反应详情

Vinyl chloroformate (56 cc) is added dropwise in the course of 10 minutes to a solution, cooled to +5° C., of (3aRS,7aRS)-2-benzyl-7,7-diphenylperhydro-4-isoindolone (193 g) in 1,2-dichloroethane (1225 cc). After stirring for 30 minutes at between 10° and 20° C., the reaction mixture is heated to reflux for 90 minutes, cooled and concentrated to dryness under reduced pressure (2.7 kPa then 1 kPa). The crystalline mass obtained is stirred vigorously 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-vinyloxycarbonylperhydro-4-isoindolone (177 g), m.p. 178° C. is obtained.

1. temperaturethe reaction mixture is heated
2. temperatureto reflux 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