Month: May 2021

Related Products of 1835-65-0, These common heterocyclic compound, 1835-65-0, name is 3,4,5,6-Tetrafluorophthalonitrile, 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.

A thermometer attached to a 100ml four-necked reactor, tetrafluorophthalonitrile (compound (5)) 6.0g (30mmol), potassium fluoride 21g (36mmol, 1.2 eq.) and acetonitrile into a 50ml, stirring under a 5 it cooled. Here, beta- naphthol (compound (a-1)) was added dropwise to 4.3g (30mmol, 1.0eq.). After the addition was completed, the mixture was reacted for 1 hour at less than 5, heated to room temperature and allowed to react for 2 hours. After the reaction, the reaction mixture was taken out by releasing the water, and filtering the precipitated solid. Resulting crude by well washing the product with isopropanol and dried to obtain the compound (4-1), 6.7g, as a white solid (yield 69percent).

Statistics shows that 3,4,5,6-Tetrafluorophthalonitrile is playing an increasingly important role. we look forward to future research findings about 1835-65-0.

Reference of 194853-86-6, These common heterocyclic compound, 194853-86-6, name is 4-Fluoro-2-(trifluoromethyl)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.

A DMSO (0.5 mL) solution of 4-fluoro-2- (trifluoromethyl) benzonitrile (0.050 g, 0.26 MMOL, 1 equiv) was treated with cesium carbonate (0.120 g, 0.37 MMOL, 1.4 equiv) and N- (cyclopropylmethyl)-N-propylamine (0.035 g, 0.31 mmol, 1.2 equiv). After 3 h at 90C, the cooled reaction was treated with H2O (1 mL), and extracted with EtOAc (3x 1 mL). Concentration was followed by radial chromatography (SIO2, 1 mm plate, 90: 10; Hex/EtOAc) to afford the title compound as a white solid (0.060 g, 81%) : 1H NMR (CDCI3, 400 MHz) 8 7.51 (d, J = 9.1 Hz, 1 H), 7.00 (d, J = 2.7 Hz, 1 H), 6.84 (dd, J = 9. 0,2. 6 Hz, 1 H), 3.34 (t, J = 7. 7 Hz, 2H), 3.24 (d, J = 6. 4 Hz, 2H), 1.63 (sex, J = 7. 5 HZ, 2H), 1.02 (sept, J = 5. 4 Hz, 1 H), 0.95 (t, J = 7. 4 Hz, 3H), 0.59 (q, J = 5. 7 Hz, 2H), 0.27 (q, J = 5. 0 Hz, 2H).

The synthetic route of 194853-86-6 has been constantly updated, and we look forward to future research findings.

Reference of 127946-77-4, 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. 127946-77-4, name is 1-Amino-1-cyclopropanecarbonitrile hydrochloride belongs to nitriles-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Example 41C) (4.83 g, 10.3 mmol, Eq: 1.00) was dissolved in acetonitrile (40 ml). HATU (7.84 g, 20.6 mmol, Eq: 2.00), DIEA (2.66 g, 3.6 ml, 20.6 mmol, Eq: 2.00) and 1- aminocyclopropane-carbonitrile hydrochloride (1.47 g, 12.4 mmol, Eq: 1.20) were added to the solution and stirred at 22C for 2 h. The reaction mixture was poured into aqueous 0.1 M HC1 (100 ml) and extracted with dischloromethane (3 x 75 mL). The organic layers were dried over Na2S04 and concentrated in vacuo. The crude material was purified by flash chromatography (silica gel, 120 g, 0% to 60% AcOEt in heptane) to yield a white solid (3.2 g; 58%). m/z = 531.9 [M-H]

The synthetic route of 1-Amino-1-cyclopropanecarbonitrile hydrochloride has been constantly updated, and we look forward to future research findings.

Related Products of 6136-68-1,Some common heterocyclic compound, 6136-68-1, name is 3-Acetylbenzonitrile, molecular formula is C9H7NO, 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 acetophenones 1-6 (16.65 mmol) in 2-Metetrahydrofuran(20 mL), copper(II)bromide (19.98 mmol)was added (Raghunath et al. 2015). The reaction mixturewas allowed to stir at room temperature for 24 h. Aftercompletion of the reaction (monitored by TLC), reactionmixture was filtered off. The filtrate containing the 2-bromo-1-phenylethanones 7-12 was taken to the next stepwithout isolation. However, to check the purity of theformed phenacyl bromides, two representative compounds(8 and 10) were isolated in standard procedure by evaporatingthe solvent under vacuum and confirmed by spectralanalysis (1H NMR, Mass, and HPLC). As all the derivativeswere pure by TLC, they were preceded to next step withoutpurification/isolation.

The synthetic route of 6136-68-1 has been constantly updated, and we look forward to future research findings.

Adding a certain compound to certain chemical reactions, such as: 67515-59-7, name is 4-Fluoro-3-(trifluoromethyl)benzonitrile, belongs to nitriles-buliding-blocks compound, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 67515-59-7, Safety of 4-Fluoro-3-(trifluoromethyl)benzonitrile

Preparation No.44: Preparation of 4-(4-fluoropiperidin-l-yl)-3- (trifluoromethyl)benzonitrile:; In a 200 mL round bottom flask, 4-fluoro-3-trifluoromethyl-benzonitrile (5.43 g, 28.7 mmol), 4-fluoropiperidine hydrochloride (4.407 g, 31.6 mmol), and potassium carbonate (9.92 g, 71.7 mmol) in DMF (50 mL) were added to give a tan suspension. The mixture was heated at about 90 C for about 40 h. After cooling to ambient temperature, the reaction mixture was partitioned between water (75 mL) and ethyl acetate (75 mL). The organic layer was washed with water (50 mL) and brine (50 mL). The organic layer was dried over anhydrous magnesium sulfate and the solvent was removed in vacuo. The crude material was purified via gradient normal phase chromatography on silica gel (0% to 100% ethyl acetate in heptane over 6 column volumes) to afford 4-(4-fluoropiperidin- 1 -yl)-3-(trifluoromethyl)benzonitrile (4.87 g, 17.9 mmol, 62% yield). LC/MS Rf = 7.51 min.; MS m/z : (M+H+AcOH)+. (Table 1, Method n). .H NMR (400 MHz, DMSO-4) ppm 8.17 (d, J = 1.98, 1H), 8.06 (dd, J = 2.01, 8.51, 1H), 7.59 (d, J= 8.53, 1H), 4.87 (tdd, J = 3.26, 6.66, 48.35, 1H), 3.13 (t, J= 10.01, 2H), 3.02-2.92 (m, 2H), 2.07-1.78 (m, 4H).

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, 4-Fluoro-3-(trifluoromethyl)benzonitrile, other downstream synthetic routes, hurry up and to see.

Synthetic Route of 5414-21-1, 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. 5414-21-1, name is 5-Bromovaleronitrile belongs to nitriles-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

[0526] To a stirred solution of [1-(2-(trimethylsilyl)ethoxymethyl)-(1H-benzimidazol-2-ylmethyl)]-(5,6,7,8-tetrahydro-quinolin-8-yl)-amine (188 mg, 0.455 mmol) and diisopropylethyl amine (0.26 ml<1.49 mmol) in CH3CN was added 5-bromovaleronitrile (0.12 mL, 1.03 mmol). The mixture was heated at 80 C. for 47 hours, after which time the reaction was cooled to room temperature. After removal of volatiles under reduced pressure, the residue was dissolved in CH2Cl2 (20 mL). The solution was washed with brine (3×15 mL). The aqueous phase was extracted with CH2Cl2 (1×15 mL). The combined organic phases were dried (Na2SO4), filtered and concentrated under reduced pressure to give a crude orange oil (306 mg). Purification of this oil by column chromatography (1.75 cm OD, 14 g silica, 40:1 CH2Cl2: CH3OH) afforded the purified tertiary amine (110 mg, 50%). [0527] The amine from above (110 mg) was dissolved in ammonia saturated CH3OH(12 mL) and treated with Raney-Nickel (410 mg). The mixture was shaken on a Parr hydrogenator at 50 psi H2 for 20 hours, after which time the mixture was filtered through celite and concentrated to give a crude yellow-orange oil (124 mg). [0528] The amine from above (124 mg) was dissolved in 4N HCl (2 mL) and heated to 50 C. for 6 hours. The mixture was then cooled to room temperature and basified with 10N NaOH (final pH>13). This aqueous phase was extracted with CH2Cl2 (4×10 mL). The organic phase was then dried (Na2SO4), filtered and concentrated to give a crude brown foam (83 mg). Purification of this foam by radial chromatography on silica gel (40:1:1 CH2Cl2: CH3OH: NH4-OH) afforded the pure freebase (38 mg, 46% over two steps). [0529] Using the General Procedure D: Conversion of the freebase from above (38 mg) to the hydrobromide salt gave COMPOUND 50 as a white solid (53 mg, 76%). 1H NMR (D2O) delta 1.14-1.28 (m, 2H), 1.39-1.57 (m, 4H), 1.77-1.90 (m, 1H), 1.96-2.10 (m, 1H), 2.13-2.23 (m, 1H), 2.31-241 (m, 1H), 2.46-2.57 (m, 1H), 2.73-2.90 (m, 3H), 2.96-3.03 (m, 2H), 4.38 (d, 1H, J=16.7 Hz), 4.47-4.57 (m, 2H), 7.60 (dd, 2H, J 6.3, 3.3 Hz), 7.80 (dd, 2H, J=6.2, 3.1 Hz), 7.86 (dd, 11H, J=7.9, 6.0 Hz), 8.31 (d, 1H, J=7.0 Hz), 8.62 (d, 1H, J=4.7 Hz). 13C NMR (D2O) delta 20.40, 23.88, 26.92, 27.63, 27.87, 39.68, 48.51, 52.09, 60.86, 114.26 (2 carbons), 125.85, 126.83 (2 carbons), 131.17, 139.29, 140.47, 147.92 (2 carbons), 151.48, 152.00. ES-MS m/z 364 (M+H) Anal Calc. for C22H29N5 3.1HBr 2.6H2O: C, 39.97; H, 5.69; N, 10.59; Br, 37.46. Found: C, 39.96; H, 5.64; N, 10.62; Br, 37.36.

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

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. 60702-69-4, name is 2-Chloro-4-fluorobenzonitrile, This compound has unique chemical properties. The synthetic route is as follows., Application In Synthesis of 2-Chloro-4-fluorobenzonitrile

Reference Example 112 N-(3-chloro-4-cyanophenyl)-4-fluorophenylalanine To a solution of 2-chloro-4-fluorobenzonitrile (1.8 g) in dimethyl sulfoxide (30 mL) were added 4-fluorophenylalanine (2.54 g) and cesium carbonate (4.90 g), and the mixture was stirred at 90 C. overnight. After allowing to room temperature, ethyl acetate was added, and the mixture was extracted twice with saturated aqueous sodium hydrogen carbonate solution. The aqueous layers were combined, and acidified with citric acid, and the mixture was extracted twice with ethyl acetate. The organic layers were combined, washed with saturated brine, and dried over magnesium sulfate. The solvent was evaporated under reduced pressure to give the title compound as a brown oil (yield: 3.69 g, 100%). 1H-NMR(CDCl3)delta:3.07-3.30(2H,m), 4.40(1H,q,J=5.9 Hz), 4.72(1H,d,J=6.6 Hz), 6.46(1H,dd,J=8.7,2.3 Hz), 6.60(1H,d,J=2.3 Hz), 6.94-7.05(2H,m), 7.07-7.16(2H,m), 7.41(1H,d,J=8.7 Hz).

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 60702-69-4.

Synthetic Route of 6629-04-5,Some common heterocyclic compound, 6629-04-5, name is N-Cyanoacetylurethane, molecular formula is C6H8N2O3, 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.

According to Scheme 5 Step 1: To a suspension of nitoaniline (5 g, 36.2 mmol) in concentrated HCl (9 mL) and water (50 mL) at 0 C. was added dropwise over 30 minutes a solution of sodium nitrite (5 g, 72.4 mmol in 200 mL water) the crude orange suspension was filtered at 0 C. and the obtained diazonium salt was added portionwise over 1 hour under vigorous stirring to a suspension of ethyl 2-cyanoacetate (6.22 g, 39.8 mmol) and sodium acetate (21.0 g, 257 mmol) in ethanol (200 mL). The reaction mixture was allowed to rest at 0 C. for 1 h. The mixture was filtered, washed with water then cooled ethanol and dried to afford (Z)-2-cyano-2-(2-(3-nitrophenyl)hydrazono)acetylcarbamate 9(A) (11.0 g, 100%, 75% of purity) as an orange solid. The crude solid was used in the next step without further purification.Rf=0.32 CH2Cl2/MeOH (95/5)LC1: Rt=3.65MS m/z (ES) [M+H]+=306

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route N-Cyanoacetylurethane, its application will become more common.

Reference of 77532-79-7,Some common heterocyclic compound, 77532-79-7, name is 5-Fluoro-2-methylbenzonitrile, molecular formula is C8H6FN, 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.

To a nitromethane (0.1 mL) solution of 5-fluoro-2-methylbenzonitrile (1k) (30 mg, 0.222 mmol) wereadded H2O (1.0 mL), DBU (68 mg, 0.444 mmol), copper (I) iodide (8.5 mg, 0.0444 mmol), cesium(I) carbonate (36 mg, 0.111 mmol) at room temperature. The reaction mixture was heated at 100 Cfor 3 h and then poured into water (50 mL). The organic layer was separated and the aqueous layerwas extracted with AcOEt. The combined organic layer was dried over MgSO4. The solvent wasremoved under reduced pressure. The residue was purified by preparative TLC on silica gel elutingwith AcOEt-n-hexane (1:1) to give 5-fluoro-2-methylbenzamide (2k) (20 mg, 59%) as pale yellowpowders.mp 117-119 C,

The synthetic route of 77532-79-7 has been constantly updated, and we look forward to future research findings.

Synthetic Route of 10137-67-4,Some common heterocyclic compound, 10137-67-4, name is Ethyl 3-cyanopropanoate, molecular formula is C6H9NO2, 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 suspension of Zn powder (196 mg, 3 mmol) in THF (5 mL) weresuccessively added the appropriate nitrile (1 mmol), pure or dissolvedin a minimum amount of THF, and allyl bromide (0.26 mL, 3 mmol). The solution was heated rapidly to reflux and cooled down to rt after 10-15 min. Aq 1 M HCl (5 mL) was added and the aqueous layer was extracted with EtOAc (2 × 5 mL). The combined organic layers weresuccessively washed with aq 2 M NaOH and brine, dried (anhydMgSO4), and filtered. The solvents were removed in vacuo to affordthe crude product, which was purified by flash chromatography onsilica gel, only when required.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route Ethyl 3-cyanopropanoate, its application will become more common.