2-CYANO-N-(3,4-DIMETHYL-PHENYL)-ACETAMIDE synthesis
- Product Name:2-CYANO-N-(3,4-DIMETHYL-PHENYL)-ACETAMIDE
- CAS Number:24522-42-7
- Molecular formula:C11H12N2O
- Molecular Weight:188.23
Yield:-
Reaction Conditions:
Stage #1: cyanoacetic acidwith phosphorus pentachloride in dichloromethane at 40; for 0.5 h;Cooling with ice;
Stage #2: 4-amino-o-xylene in dichloromethane at 20 - 40; for 2 h;
Steps:
1.a Step a: Synthesis of substituted 2-cyano-N-phenylacrylamide compound (22)
General procedure: A mixture of cyanoacetic acid (1.0 g) was dissolved in dichloromethane (20 ml)Ice water bath under the conditions of adding phosphorus pentachloride (2.5g),Then moved to 40 ° C for about half an hour,Cold to room temperature,The corresponding substituted aniline (40) was added,And then slowly heated to 40 ° C to continue the reaction,After 2 h the reaction was stopped and the solvent was concentrated under reduced pressure,Then add 50ml of water, a large number of solid appear,Direct filtering,The filter cake was washed with 10 ml of saturated NaHCO3 solutionAnd anhydrous ether to give the title compound instead of 2-cyano-N-phenylacrylamide (22)No further processing,The yield is about 83% -95%.
References:
CN106977474,2017,A Location in patent:Paragraph 0034; 0035; 0036
