反应详情

A mixture of 2-(5,6-dimethoxy-benzo[b]thien-2-yl)-3-methyl-2-(4-morpholinyl)-pentanedinitrile (7.4 g), glacial acetic acid (37.5 ml) and water (12.5 ml) was stirred and heated at reflux under an atmosphere of nitrogen. After 45 min. the reaction mixture was cooled and poured into crushed ice (200 g). The ice was allowed to melt and the resultant precipitate was filtered and dried at 65° C. under vacuum to give 4-(5,6-dimethoxybenzo[b]thien-2-yl)-3-methyl-4-oxo-butane nitrile as a pale yellow solid (5.2 g). A portion crystallized from dichloromethane/diethyl ether had m.p. 148°-150° C.

1. temperatureheated
2. temperatureat reflux under an atmosphere of nitrogen
3. temperatureAfter 45 min. the reaction mixture was cooled
4. additionpoured
5. filtrationthe resultant precipitate was filtered
6. customdried at 65° C. under vacuum