Gamma-Butyrolactone → HCID 701787、化合物

反応式

[F:1][C:2]([F:11])([F:10])[C:3]1[CH:4]=[C:5]([CH:7]=[CH:8][CH:9]=1)[NH2:6].[C:12]1(=O)[O:16][CH2:15][CH2:14][CH2:13]1.C1(C)C=C(C)C=C(C)C=1>O>[F:1][C:2]([F:10])([F:11])[C:3]1[CH:4]=[C:5]([N:6]2[CH2:12][CH2:13][CH2:14][C:15]2=[O:16])[CH:7]=[CH:8][CH:9]=1

参加物

反応条件

温度: 198 °C

実験手順

A reaction flask was charged with 70.0 g (0.434 mole) of m-trifluoromethylaniline and 37.4 g (0.434 mole) of butyrolactone. The mixture was heated to reflux at 198° C for 185 minutes. Then, 1.0 g (0.0058 mole) of ptoluenesulphonic acid was added, and the resulting mixture was refluxed for an additional 100 minutes, during which time the temperature dropped from 164° C to 138° C. The mixture was then cooled, a DEan-Stark trap was installed on the condenser, and 50 ml of mesitylene was added. The mixture was then refluxed at 181-187° C until water was no longer produced. The precipitate formed by the reaction was filtered out of the mixture and dried in vacuo, yielding 45.6 g of 1-(m-trifluoromethylphenyl)-2-pyrrolidone, melting point 65°-66° C.