Month: May 2021

Related Products of 1247885-41-1,Some common heterocyclic compound, 1247885-41-1, name is 5-Amino-2,3-difluorobenzonitrile, molecular formula is C7H4F2N2, 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.

5-bromo-2,3-difluorobenzonitrile (0274) At room temperature, copper bromide (6.1 g, 42.80 mmol) was added to the solution of 5-amino-2,3-difluorobenzonitrile (660 mg, 4.28 mmol) in acetonitrile (33 mL). The reaction mixture was then added dropwise by a solution of tert-butyl nitrite (4.4 g, 42.77 mmol) in acetonitrile (33 mL) over 1.5 h period at room temperature. The resulting mixture was stirred for 3 h at room temperature and then treated with water (50 mL). The resulting solution was extracted with ethyl acetate (150 mL×3). The organic phases were combined, washed with brine and dried over sodium sulfate. The solvent was removed under reduced pressure and the residue was purified by flash chromatography eluting with ethyl acetate in hexane (0% to 10% gradient) to yield 5-bromo-2,3-difluorobenzonitrile as light yellow solid (660 mg, 71%).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 5-Amino-2,3-difluorobenzonitrile, its application will become more common.

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 218632-01-0 as follows. Computed Properties of C7H3FN2O2

To a stirred solution of 3-fluoro-4-nitrobenzonitrile (1 g, 6.02 mmol) in CH2Cl2 (5 mL) under an inert atmosphere was added potassium carbonate (1.66 g, 12.05 mmol) and cyclopropanamine (3.33 mL, 48.19 mmol) drop wise at room temperature. The reaction mixture was stirred at room temperature for 4 h. After consumption of starting material (by TLC), the reaction mixture was diluted with water (30 mL) and extracted with EtOAc (2*40 mL). The combined organic extracts were dried over anhydrous Na2SO4 and concentrated under reduced pressure to afford 3-(cyclopropylamino)-4-nitrobenzonitrile (900 mg, 4.43 mmol, 74%) as yellow solid. 1H NMR (400 MHz, CDCl3): delta 8.24 (d, J=8.7 Hz, 1H), 8.07 (br s, 1H), 7.64 (d, J=1.7 Hz, 1H), 6.93 (dd, J=8.7, 1.7 Hz, 1H), 2.62-2.57 (m, 1H), 1.03-0.97 (m, 2H), 0.72-0.67 (m, 2H). LC-MS: m/z 201.9 [M-H]+ at 3.25 RT (99.61% purity).

According to the analysis of related databases, 218632-01-0, the application of this compound in the production field has become more and more popular.

Adding a certain compound to certain chemical reactions, such as: 50670-64-9, name is 5-Amino-2-methylbenzonitrile, 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 50670-64-9, Product Details of 50670-64-9

General procedure: mixture of 4-chloroquinazolines derivatives 10a-10j(5 mmol) and substituted anilines (6 mmol) in isopropanol(45 mL) was stirred at reflux for 3 h. The reaction mixture wascooled to room temperature and the resultant precipitate was collectedby filtration. The solid was further dried in vacuum to givethe compounds a-j.

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Synthetic Route of 4640-66-8,Some common heterocyclic compound, 4640-66-8, name is 4-Chlorophenacylcyanide, molecular formula is C9H6ClNO, 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: A microwave tube was charged with ketonitrile (2.0 mmol), methanol (1 mL), and hydrazine monohydrate (2.6 mmol) and subjected to microwave irradiation (100 W, 150 C) for 5 minutes. Volatiles were subsequently removed under reduced pressure. The residue was purified by either trituration with cold methanol or cyclohexane, or by using column chromatography to give the final product.

The synthetic route of 4640-66-8 has been constantly updated, and we look forward to future research findings.

Reference of 76469-88-0,Some common heterocyclic compound, 76469-88-0, name is Methyl 4-(cyanomethyl)benzoate, molecular formula is C10H9NO2, 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 solution of methyl 4-(cyanomethyl)benzoate (9.5 g, 54.2 mmol) in ethanol (100 mL), hydroxylamine hydrochloride (6.78 g, 98 mmol) and sodium bicarbonate (8.20 g, 98 mmol) were added. The resulting reaction mixture was stirred at 65 oC for 18 h. The reaction mixture was filtered and the filtrate was concentrated under reduced pressure to obtain methyl-4-(2-amino-2- (hydroxyimino)ethyl)benzoate (11.2 g, 53.8 mmol, 99 % yield).

The synthetic route of 76469-88-0 has been constantly updated, and we look forward to future research findings.

Electric Literature of 96606-37-0, 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 96606-37-0 as follows.

2,4,6-trifluorobenzonitrile (100 mg, 64 mmol), phenol (120 mg, 1.2 mmol) and potassium carbonate (87 mg, 64 mmol) were irradiated in the microwave in NMP (3 mL) at 120C for 10 minutes at which point LCMS indicated that the reaction was complete. Guanidine carbonate (231 mg, 1.91 mmol) was added and the reaction irradiated in the microwave at 150C for 15 minutes. The mixture was cooled and purified directly by reversed phase HPLC (15 to 95% ACN in DI water containing 0.1% TFA: 15 minute gradient). The pure fractions were pooled and concentrated to afford the product as an off white solid.135 mg, 61% yield, 2 steps.1H-NMR (300 MHz, DMSO d6) delta 12.68 (s, 1H), 8.93 (s, 1H), 8.40 (bs, 2H), 7.54-7.43 (m, 6H), 7.37-7.28 (m, 2H), 7.15 (d, 2H, J=7.2 Hz), 6.42 (s, 1H), 6.01 (s, 1H). LC/MS [M+H]+ 345.4.

According to the analysis of related databases, 96606-37-0, the application of this compound in the production field has become more and more popular.

Application of 89642-49-9, These common heterocyclic compound, 89642-49-9, name is 4-Bromo-3-nitrobenzonitrile, 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 for Silyl Acetylenes (61 b,e,f). Cul (2 mol %) was added to a stirred mixture of an aryl halide 60, (trimethylsilyl)acetylene (min. 1.3 equiv), and PdCl2(PPh3)2 (2 mol %) in triethylamine. See . The mixture was heated at 60 C until the reaction was complete (ca. 3 h). Salts were filtered off and washed with EtOAc. Combined filtrates were evaporated under reduced pressure, and the residue was purified by column chromatography eluding with hexane/EtOAc. The recovered material was recrystallized as necessary. 3-nitro-4-[2-(trimethylsilyl)ethynyl]benzonitrile (61 b) was prepared from aryl bromide 60b as an off-white solid (1.61 g, 66%): mp 81-82 C (toluene/hexane); 1H NMR delta 8.69 (d, J = 1.6 Hz, 1H), 8.20 (dd, J = 8.0 and 1.6 Hz, 1H), 7.94 (d, J = 8.2 Hz, 1H), 0.27 (s, 9H); HPLC (Method B) tR 8.39 min (100 area % at 254 nm). Anal. (C12H12N2O2Si) C, H, N. A second general method is depicted in Scheme 2 immediately hereinabove and comprises the cycloaddition of cyanophenylacetylenes 51 and benzaldehyde chlorooximes 52 in the presence of bis(tributyltin) oxide, see Moriya, O., et al., J. Chem. Soc., Perkin Trans., 1, 413-417 (1994); Moriya, O., et al., J. Chem. Soc., Chem. Commun., 17-18 (1991), or triethylamine, see Thomsen, l., et al., Acta Chem. Scand. (B), 319-313 (1988), in nonpolar solvents to give isoxazole dinitriles 53a-h,k-s and bromonitrile 53i. The latter was treated with copper(I) cyanide to give dinitrile 53j. See Friedman. L., et al., J. Org. Chem., 26, 2522-2524 (1961). This method also afforded alternate routes to dinitriles 50a,b,g, k prepared by the first method as provided in Scheme 1. The phenylacetylene synthons 51a-g were prepared as shown in Scheme 3 below. Starting materials 60a,e,g were commercially available. Nitration of 60a gave 60b. See Borsche, W., L., et al., Chem. Ber., 49, 2222-2243 (1916). The latter was reduced to aniline 56, see Blanksma, J. J., et al., Recl. Trav. Chim. Pays-Bas, 66, 365-373 (1947), which underwent diazotization followed by treatment with copper(l) chloride to give chlorobenzene 60c. Triflate 60d was prepared by treatment of 4-bromo-3-hydroxybenzonitrile with triflic anhydride. The preparation of aryl iodide 60f began with the known transformation of aldehyde 57 to iodo derivative 58. See Lulinski, P., et al., Bull. Chem. Soc. Jpn., 73(4), 951-956 (2000). Treatment of 58 with hydroxylamine hydrochloride gave aldoxime 59, which was dehydrated to give nitrile 60f using acetic anhydride. The aryl halides or triflates 60a-g were treated with (trimethylsilyl)acetylene, see Roesch. K. R., et al., J. Org. Chem., 66, 412-420 (2001), or with 2-methyl-3-butyn-2-ol, see Bleicher, L. S., et al., J. Org. Chem., 63, 1109-1118 (1998), to give intermediates 61a-f or 62a-f, respectively, of which 61a,d and 62a have been reported previously. See Dirk. S. M., et al., Tetrahedron, 59(3), 287-293 (2003); Bleicher, L. S., et al., J. Org. Chem., 63, 1109-1118 (1998). The acetylenes 51 (of which 51a,e were known previously), see Blackburn, B. K., et al., J. Med. Chem., 40(5), 717-729 (1997); Dulog, L., et al., Liebigs Ann. Chem., 9, 1663-1671 (1995), were obtained by the treatment of intermediates 61 or 62 with cesium carbonate in acetonitrile or sodium hydride in toluene, respectively. See Bleicher, L. S., et al., J. Org. Chem., 63, 1109-1118 (1998). The use of cesium carbonate in acetonitrile was introduced for the deprotection of intermediates 61 after the treatment of compound 61b with potassium carbonate in methanol, see Blackburn, B. K., et al., J. Med. Chem., 40(5), 717-729 (1997), failed to give product 51b. The pathway using 2-methyl-3-butyn-2-ol provided more economical preparations of all phenylacetylenes 51 except nitro analog 51b. ; Reagents and conditions: (a) fuming HNO3, H2SO4; (b) Fe, AcOH, EtOH; (c) NaNO2, aq. HCl, then CuCl; (d) NalO4, l2, AcOH, AC2O, H2SO4; (e) NH2OH HCl, Py, EtOH (f) Ac2O; (g) TMSA, Pd2Cl2(PPh3)2, Cul, Et3N; (h) TMSA, PPh3, Pd(PPh3)4, Cul, piperidine; (j) 2-methyl-3-butyn-2-ol, Pd2Cl2(PPh3)2, Cul, Et3N; (k) 2-methyl-3-butyn-2-ol, 10% Pd/C, PPh3, Cul, aq. K2CO3/DME; (I) Cs2CO3, aq. CH3CN or MeOH; (m) NaH, toluene.

Statistics shows that 4-Bromo-3-nitrobenzonitrile is playing an increasingly important role. we look forward to future research findings about 89642-49-9.

Reference of 2920-38-9, 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. 2920-38-9, name is [1,1′-Biphenyl]-4-carbonitrile belongs to nitriles-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

General procedure: 1800 muL (90%) Tris buffer (50 mM, pH 7.6) and 200 muL(10%) of methanol or acetone. In a 2 mL Eppendorf, NHase (10 mg) was added followed by Trisbuffer. Nitrile substrate (10 mg dissolved in 200 muL methanol or acetone) was added to the 2 mLEppendorf tube. (If an amine group was present on the nitrile substrate a Tris buffer of pH 9 wasused). The reaction mixture was incubated at 30 C on an ESCO Provocell microplateshaker/incubator (Esco Technologies, Halfway House, South Africa) (199 rpm). The reaction wasallowed to proceed for 24 h, 48 h or 5 d, depending on conversion, as monitored by TLC analysis.Ethyl acetate and water were added to the reaction mixture, and after separation, the organic layerwas concentrated under reduced pressure, and the resulting mixture was then purified by silica gelcolumn chromatography eluting with 20% to 90% ethyl acetate/ hexane.

The synthetic route of [1,1′-Biphenyl]-4-carbonitrile has been constantly updated, and we look forward to future research findings.

Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 6629-04-5, name is N-Cyanoacetylurethane, A new synthetic method of this compound is introduced below., Computed Properties of C6H8N2O3

General procedure: To the mixture of substituted anilines (0.08mol), concentrated hydrochloric acid (45.0mL) and water (120.0mL), aqueous solution of NaNO2 (60.0mL, 0.11mol) was added drop-wise under stir at a rate that the temperature below 0C, and the reaction mixture was stirred for 0.5h. A mixture of ethyl (2-cyanoacetyl)carbamate (13.7g, 0.09mol) and sodium acetate (24.0g, 0.27mol) in ethanol (400.0mL) was added drop-wise to the resulting diazonium salt solution below 0C and stirred for a further 2h. The precipitate was collected by filtration and washed with water (40.0 mL×2), dried to give compounds 7a-f.

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.

Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 108168-88-3, name is N-(tert-Butyl)-2-cyanoacetamide, A new synthetic method of this compound is introduced below., Safety of N-(tert-Butyl)-2-cyanoacetamide

To a 10 ml sealed tube, N-((2S,3R)- l-(((S)-l-((2-fluoro-4-methylbenzyl)amino)-3-(3- formylphenoxy)-l – oxopropan -2-yl)amino)-3-hydroxy-l -oxobutan-2-yl)-5-methylisoxazole-3- carboxamide (1 10 mg, 0.2 mmol) and N-(tert-butyl)-2-cyanoacetamide (85.5 mg, 0.61 mmol) were dissolved in methanol (2 ml). Piperidine (2 drops) was added to the reaction mixture and stirred at 80 C for 1 h. Water was added and the product was extracted with ethyl acetate, the combined organic later was dried over sodium sulfate, filtered and concentrated. The crude material was purified using flash chromatography and further triturated with diethyl ether to yield 30 mg of the title compound. LC-MS (ES, m/z): 663 [M+H

The synthetic route of 108168-88-3 has been constantly updated, and we look forward to future research findings.