反应详情

Phosphorus pentachloride (27.2 g.) was added portionwise during ca. 20 minutes to a stirred and cooled (ice-bath) suspension of 2-dichloroacetoxyimino-2-(thien-2-yl)acetic acid (syn-isomer) (37.0 g.) in methylene chloride (370 ml.). The mixture was stirred at 0° for a further 30 minutes during which time all the solid dissolved. After removal of the solvent under reduced pressure, benzene was evaporated from the residue at 20°, and the process repeated to give 2-dichloroacetoxyimino-2-(thien-2-yl)acetyl chloride (syn-isomer) as an oil that was used directly in the next stage.

1. temperaturecooled
2. stirringThe mixture was stirred at 0° for a further 30 minutes during which time all the solid
3. dissolutiondissolved
4. customAfter removal of the solvent under reduced pressure, benzene
5. customwas evaporated from the residue at 20°