Preparation method of amide compound
A technology of dehydration and condensation of amide compounds, applied in the preparation of organic compounds, carboxylic acid amide preparation, chemical instruments and methods, etc., can solve the problems of high cost of coupling reagents, many chemical wastes, cumbersome procedures, etc., and achieve easy separation Purification, broad substrate range, and simple operation
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[0023] Example 1
[0024] Method for preparing a lactam compound of the following reaction formula:
[0025]
[0026] Specific steps are as follows:
[0027] 100mL pressure bottle was added to diethylamine (10mmol), benzoic acid (30mmol), sodium hydroxide (30mmol), bromo-sulfonyl fluoride (15mmol), acetonitrile (25mL), at reflux in an oil bath at 50 deg.] C for 18 h, after completion of the reaction, the reaction solution was added 30mL 1M sodium hydroxide solution and then extracted three times with 20mL ethyl acetate, the extract was washed with 20mL 1M hydrochloric acid solution and then dried over anhydrous sodium sulfate and evaporated under reduced pressure, to give the white solid N, N- diethyl-fluoro-benzamide (1.41g, 80% yield).
[0028] Hydrogen spectrum data of this compound obtained in Example amides embodiment is as follows: 1 H-NMH (500MHz, CDCl 3 ) Δ = 7.40-7.36 (m, 5H), 3.56 (s, 2H), 3.26 (s, 2H), 1.26 (s, 3H), 1.11 (s, 3H).
Example Embodiment
[0029] Example 2
[0030] Method for preparing a lactam compound of the following reaction formula:
[0031]
[0032] Specific steps are as follows:
[0033] Was added aniline (10mmol) to a 100mL pressure bottle, o-trifluoromethyl benzoic acid (30mmol), sodium hydroxide (30mmol), bromo-sulfonyl fluoride (15mmol), acetonitrile (25 mL), at 50 deg.] C oil bath under reflux for 18 h, after completion of the reaction, the reaction solution was added 30mL 1M sodium hydroxide solution and then extracted three times with 20mL ethyl acetate. the extract was washed with 20mL 1M hydrochloric acid solution and then dried over anhydrous sodium sulfate Save pressure distillation, to obtain a white solid N- phenyl-2- (trifluoromethyl) benzamide (2.20g, 83% yield).
[0034] Hydrogen spectrum data of this compound obtained in Example amides embodiment is as follows: 1 H-NMH (500MHz, DMSO-d 6 ) Δ = 10.55 (s, 1H), 7.85 (d, J = 7.6Hz, 1H), 7.80 (t, J = 7.3Hz, 1H), 7.73-7.70 (m, 4H), 7.36 (t, J = 7.6 h
Example Embodiment
[0035] Example 3
[0036] Method for preparing a lactam compound of the following reaction formula:
[0037]
[0038] Specific steps are as follows:
[0039] Was added L- valine ethyl ester (10mmol) to a 100mL pressure bottle, benzoic acid (30mmol), sodium hydroxide (30mmol), bromo-sulfonyl fluoride (15mmol), acetonitrile (25 mL), at 50 deg.] C oil after the reaction was refluxed for 18 h at a bath, after completion of the reaction, the reaction solution was added 30mL 1M sodium hydroxide solution and then extracted three times with 20mL ethyl acetate, the extract was washed with 20mL 1M hydrochloric acid solution and then dried over anhydrous sodium sulfate evaporated under reduced pressure to obtain a white solid benzoyl -L- valine ethyl ester (2.17g, 87% yield, 99% ee).
[0040] Hydrogen spectrum data of this compound obtained in Example amides embodiment is as follows: 1 H-NMR (500MHz, CDCL 3 ) Δ = 7.81 (d, J = 7.3Hz, 2H), 7.50 (t, J = 7.3Hz, 1H), 7.44 (t, J = 7.5Hz, 2H), 6.68
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