反应详情

Vinyl chloroformate (56 cc) is added dropwise in the course of 10 minutes to a solution of (3aRS,7aRS)-2-benzyl-7,7-diphenyl-4-perhydroisoindolone (193 g) in 1,2-dichloroethane (1,225 cc) cooled to +5° C. After stirring for 30 minutes at between 10° and 20° C., the reaction mixture is refluxed for 90 minutes, cooled and concentrated to dryness under reduced pressure (2.7 kPa then 1 kPa). The crystalline mass obtained is pounded with cold isopropyl ether (200 cc). The crystals obtained are drained, washed with isopropyl ether (2 * 100 cc) and dried. (3aRS,7aRS)-7,7-diphenyl-2-vinyloxycarbonyl-4-perhydroisoindolone (177 g) melting at 178° C. is obtained.

1. temperaturecooled to +5° C
2. temperaturethe reaction mixture is refluxed for 90 minutes
3. temperaturecooled
4. concentrationconcentrated to dryness under reduced pressure (2.7 kPa
5. customThe crystalline mass obtained
6. customThe crystals obtained
7. washwashed with isopropyl ether (2 * 100 cc)
8. customdried