Tag: M.W=100-200

Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 6136-68-1, name is 3-Acetylbenzonitrile, This compound has unique chemical properties. The synthetic route is as follows., Formula: C9H7NO

Part A. Preparation of ethyl 3-(3-cyanophenyl)-3-oxopropionate. To a suspension of sodium hydride (1.2 g of 60% suspension in mineral oil, hexane-washed, 30.3 mmol) in 40 mL of tetrahydrofuran was added diethyl carbonate (3.7 mL, 30.3 mmol) and 3-acetyl benzonitrile (2.2 g, 15.2 mmol). The resulting suspension was stirred at 65 C for 1 h and then was cooled to room temperature. There was added 40 mL of 10% aqueous HCl and the reaction mixture was diluted with ethyl acetate and the layers were separated. The organic layer was washed with brine, dried (MgSO4) and concentrated in vacuo to afford 3.2 g (96%) of the title compound, which was sufficiently pure to be used without purification. MS (NH3-CI) 218.3 (M+H)+.

Chemical properties determine the actual use. Each compound has specific chemical properties and uses. We look forward to more synthetic routes in the future to expand reaction routes of 6136-68-1.

Electric Literature of 17417-09-3, In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 17417-09-3, name is 2-Fluoro-5-nitrobenzonitrile belongs to nitriles-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

To 2-fluoro-5-nitrobenzonitrile (5.00 g, 30.1 mmol) in DMF (100 mL), triethylamine (9.30 mL, 66.7 mmol) was added and followed by ethanethiol (2.80 mL, 37.9 mmol). After stirring at rt for 1 h, the reaction mixture was poured into water (500 mL). The resulting precipitate was filtered and dried on high vacuum overnight to provide Intermediate 9A (6.08 g, 97%).

The synthetic route of 2-Fluoro-5-nitrobenzonitrile has been constantly updated, and we look forward to future research findings.

Synthetic Route of 52798-01-3, These common heterocyclic compound, 52798-01-3, name is Methyl (4-cyanophenyl)acetate, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

Concentrated hydrochloric acid (37%, 259 mg) was added dropwise to a mixture of methyl 2- (4-cyanophenyl) acetate (3.2 g, 18.3 mmol) and10% palladium on carbon catalyst (175 mg) in 50 ml of methanol.Hydrogen gas was bubbled in and stirred for 12 hours at room temperature.Excess catalyst was removed by filtration and the organic phase was distilled off under reduced pressure.The filtrate was concentrated under reduced pressure. The residue was dissolved in ethyl acetate (50 mL), washed with brine, dried and concentrated. The residue was purified by column chromatography (methylene chloride / methanol = 20/1) to give the title compound 2.29 g (70%).

Statistics shows that Methyl (4-cyanophenyl)acetate is playing an increasingly important role. we look forward to future research findings about 52798-01-3.

Related Products of 21803-75-8, In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 21803-75-8 as follows.

The starting material was prepared as follows: sodium hydride (2.7 g, 67.5 mmol) was suspended in NMP (75 ml) and benzyl alcohol (7.3 g, 67.6 mmol) was added over 10 minutes.. When the addition was complete the solution was stirred at 50 C. for 30 minutes. 4-Amino-3-chlorobenzonitrile (10.3 g, 67.5 mmol), (Synthesis 1985, 669), was added and the mixture was heated at 120-130 C. for 4 hours.. After cooling to ambient temperature the mixture was partitioned between water and ether.. The ether extracts were washed with brine, dried (MgSO4), the insoluble materials were removed by filtration and the volatiles were removed by evaporation.. The crude product was purified by flash chromatography eluding with ether/isohexanes (1/1 increasing to 1/0).. The purified product was recrystallized from ethyl acetate/isohexanes to give 4-amino-3-benzyloxybenzonitrile (4.7 g, 31%). 1H NMR Spectrum,; (DMSOd6) 5.10 (s, 2H); 6.10 (s, 2H); 6.20 (d, 1H); 6.35 (s, 1H); 7.25 (d, 1H); 740 (m, 5H); MS-ESI: 225 [MH]+.

According to the analysis of related databases, 21803-75-8, the application of this compound in the production field has become more and more popular.

These common heterocyclic compound, 222978-02-1, name is 2-Fluoro-4-(hydroxymethyl)benzonitrile, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route. Formula: C8H6FNO

Step D Preparation of 4-Bromomethyl-2-fluoro-benzonitrile N-Bromosuccinimide (6.6 g, 0.037 mol) was dissolved in CH2Cl2 (150 mL), cooled to 0 C. and treated with dimethylsulfide (3.27 mL, 0.0446 mol). The solution was cooled to -20 C. then treated dropwise with a solution of 2-fluoro-4-hydroxymethylbenzonitrile, as described in Step C above, (3.74 g, 0.0248 mol) in CH2Cl2 (30 mL). After the addition, the reaction mixture was stirred at 0 C. for 2 h then left to warm to ambient temperature overnight. The reaction mixture was added to ice/H2O, extracted with EtOAc, the organic layer separated, washed with brine and dried (MgSO4). Filtration and concentration to dryness gave the title compound which was purified after chromatography (silica gel, 5-10% EtOAc/hexane). 1H NMR (CDCl3) delta 7.61 (dd, 1H, J=8, 8 Hz), 7.26-7.30 (m, 2H), 4.45 (s, 2H).

The synthetic route of 2-Fluoro-4-(hydroxymethyl)benzonitrile has been constantly updated, and we look forward to future research findings.

Related Products of 4640-67-9, A common heterocyclic compound, 4640-67-9, name is 3-(4-Fluorophenyl)-3-oxopropanenitrile, molecular formula is C9H6FNO, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

General procedure: To a 10 mL of sealed vial was added benzoyl acetonitrile derivatives 1 (0.5 mmol), malononitrile (0.55 mmol), SeO2 (42.6mg, 0.38 mmol), benzoic acid (30.5 mg, 0.25 mmol), CH3CN (2 mL) and a magnetic stir bar. The reaction mixture was stirred at room temperature for 12 h. The reaction mixture was filtered, and the residue was extracted with dichloromethane (3 × 15 mL). The combined organic phases was washed with brine (45 mL), dried over anhydrous Na2SO4, and concentrated in vacuo. The residue was purified by flash column chromatograph on silica gel to afford the desired product.

The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.

Reference of 23842-82-2,Some common heterocyclic compound, 23842-82-2, name is 2-Amino-5-methoxybenzonitrile, molecular formula is C8H8N2O, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

General procedure: To a solution of the appropriate amine (X1 NH2, 100 mumomicronIota) in anhydrous pyridine (600 muL) was added a 1.2M solution of the appropriate sulfonyl chloride in anhydrous pyridine (100 muL, 120 mumomicronIota) followed by DMAP (2 mg, 20 mumomicronIota). The reaction mixture was shaken at 30C for 2 hours followed by 60C for 16 hours before concentrating in vacuo and purifying by one of the four preparative HPLC methods described below. The organic gradient used for each compound is described in the following table. Preparative HPLC Method A: Phenomenex Gemini C18 250 x 21 .2 mm, 8 mum; mobile phase A: MeCN, mobile phase B: 0.225% formic acid in water. Gradient time 8 mins; flow rate 30 mL/min. Preparative HPLC Method B: Waters Sunfire C8 150 x 30 mm, 5 mum; mobile phase A: MeCN, mobile phase B: 0.225% formic acid in water. Gradient time 8 mins; flow rate 40 mL/min. Preparative HPLC Method C: YMC-Actus Triart C18 150 x 30 mm, 5 mum; mobile phase A: MeCN, mobile phase B: 0.225% formic acid in water. Gradient time 9 mins; flow rate 30 mL/min. Preparative HPLC Method D: Agela DuraShell C18 150 x 21.2 mm, 5 mum; mobile phase A: MeCN, mobile phase B: 0.225% formic acid in water. Gradient time 10 mins; flow rate 30 mL/min. The retention times quoted in the table below were obtained using one of the following three LCMS methods: LCMS Method A: XBRIDGE 50 x 2.1 mm, 5 mum; mobile phase A: 0.0375%TFA in water; mobile phase B: 0.01875% TFA in MeCN; gradient from 1 % B to 5% B at 0.60 mins, further to 100% B at 4.00 mins and finally returning to 1 % B at 4.30-4.70 mins; flow rate 0.8 mL/min. LCMS Method B: XBRIDGE 50 x 2.1 mm, 5 mum; mobile phase A: 0.0375%TFA in water; mobile phase B: 0.01875% TFA in MeCN; gradient from 10% B to 100% B at 4.00 mins and finally returning to 1 % B at 4.30-4.70 mins; flow rate 0.8 mL/min. LCMS Method C: XBRI DGE 50 x 2.1 mm, 5 mum; mobile phase A: 0.05%NH4OH in water; mobile phase B: 100% MeCN; gradient from 5% B to 100% B at 3.40 mins, hold at 100% B to 4.20 mins and finally returning to 5% B at 4.21 -4.70 mins; flow rate 0.8 mL/min. The compounds of Examples 130-175 were prepared according to the method described for Library Protocol 3 using either 2-cyanobenzensulfonyl chloride or 2-(trifluoromethyl)benzenesulfonyl chloride and the appropriate amine as described below. Where stated the title compounds were isolated as formate salts.

The synthetic route of 23842-82-2 has been constantly updated, and we look forward to future research findings.

Application of 41171-91-9, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 41171-91-9 name is 3-Oxocyclopentanecarbonitrile, This compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.

EXAMPLE 34 N-3-cyanocyclopentyl-4-(2-(3-amino-phenoxy)ethyl)morpholine 4-(2-(3-aminophenoxy)ethyl)morpholine (2.15 g, 9.67 mmol) and 3-cyanocyclopentanone (1.06 g, 9.67 mmol) (prepared according to the process described by Della, E.; Knill, A.; Aust. J. Chem.; 47; 10; 1994; 1833-1842) were combined in 1% AcOH /MeOH (50 ml). To this solution was added NaBH3CN (925 mg, 14.5 mmol) in portions. After 12 h, the solvent was evaporated off and the residue partitioned between saturated NaHCO3 and ethyl acetate. The aqueous layer was extracted with ethyl acetate, the combined organic layers were dried over MgSO4 and evaporated down. The title compound was purified by flash chromatography with ethyl acetate as the eluent, 2.1 g MS (MH+) 316.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 3-Oxocyclopentanecarbonitrile, and friends who are interested can also refer to it.

In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 83101-12-6, name is 4-(3-Hydroxypropyl)benzonitrile belongs to nitriles-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. HPLC of Formula: C10H11NO

Example 5: Preparation of further compounds according to the invention.Amidine compounds 8 were synthesised as described by Powers et al. (scheme 2), but we used the procedure with Cu(OTf)2 to prepare the diphenyl phosphonate (20) (Jackson, S. D.; Fraser, S. A.; Ni, L.-M. ; Kam, C-M . ; Winkler, U. ; Johnson, D. A.; Froelich, C. J.; Hudig, D.; and Powers, J. C. Synthesis and Evaluation of Diphenyl Phosphonate Esters as Inhibitors of the Trypsin-like Granzymes A and K and Mast Cell Tryptase. J. Med. Chem., 1998, 41 , 2289-2301). Z-(4-AmPhGly)p(OPh)2 was prepared by a Lewis acid catalyzed amidoalkylation reaction, starting with cyanobenzaldehyde (18a) to give Z-(4- CN-PhGly)p(OPh)2 (20a) which was converted to the amidine (8a) using a Pinner type reaction. The 4-amidinophenylalanine phosphonate diphenyl ester derivative Z-(4- AmPhe)p(OPh)2 was synthesised in the same way from 4-cyanophenylacetaldehyde. 4- EPO Cyanophenylacetaldehyde (18b) was made from 4-cyanobenzaldehyde using a Darzen condensation (scheme 3). 4-(3-Oxo-propyl)-benzonitrile (18c) was synthesised from cyanobenzaldehyde: a Wittig olefination between 4-cyanobenzaldehyde and triphenylphosphoranylidene acetic acid ethyl ester followed by a reduction with NaBH4 afforded 3-(4-cyanophenylpropanol) (21) (Baraldi, G. P.; Cacciari, B.; Romagnoli, R.; Spalluto, G.; Monopoli, A.; Ongini, E. ; Varani, K. and Borea, P. A. 7-Substituted 5-Amino- 2-(2-furyl)pyrazolo[4,3-e]-1 ,2,4-triazolo[1 ,5-c]pyrimidines as A2A Adenosine Receptor Antagonists: A study on the Importance of Modifications at The Side Chain on the Activity and Solubility. J. Med. Chem., 2002, 45, 115-126). This alcohol is oxidised with the Dess Martin reagent to aldehyde 18c.Diphenyl 1-(lambda/-benzyloxycarbonylamino)-1-(4-cyanophenyl)propanephosphonate (20c)3-(4-cyanophenyl)propanol was oxidised with the dess-martin reagent to the aldehyde.The crude product was immediately dissolved in DCM without any further purification. The modified birum Oleksyszin reaction was used to prepare the diphenyl phosphonate. The obtained product was purified with flashchromatography.21percent yield starting from 3-(4-cyanophenyl)propanol1H NMR (CDCI3, 400 MHz); delta 2.1 (m, 1H), 2.35 (m, 1 H), 2.8 (m, 1 H), 2.9 (m, 1H), 4.5 (m,1H), 5.1 (m, 2H), 5.7 (d, 1 H), 7.1-7.4 (m, 16H), 7.5 (m, 3H) MS (ESI) : m/z M+1 = 527

The synthetic route of 83101-12-6 has been constantly updated, and we look forward to future research findings.

Related Products of 13388-75-5, The chemical industry reduces the impact on the environment during synthesis 13388-75-5, name is 2-(3,5-Dimethoxyphenyl)acetonitrile, I believe this compound will play a more active role in future production and life.

2-(3,5-dimethoxyphenyl)acetonitrile (100 g, 564 mmol, Eq: 1.00) was disolved in THF (500 mL). The solution was cooled to 0C and iodomethane (324 g, 142 mL, 2.26 mol, Eq: 4.0) was added. 1 M Potassium tert-butoxide solution in THF (1.69 L, 1.69 mol, Eq: 3) was added dropwise at 0C-2C over 60 min (conversion > 99% by GC after end addition). After 1 h at 0C, the reaction mixture was added to a stirred mixture of MTBE (1.5 L) and water (750 mL). The organic phase was separated, washed twice with 25% aqueous NaCl (750 mL), dried over Na2S04, filtered and concentrated under reduced pressure to give 115.8 g of the title compound as an oil (98.5a% by GC).

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles, 2-(3,5-Dimethoxyphenyl)acetonitrile, other downstream synthetic routes, hurry up and to see.