反应详情

A suspension of 10 g of 5-chloroisatin in 150 ml of THF is cooled to +4° C., 220 ml of a 1M solution of benzylmagnesium chloride in ether are added dropwise and the mixture is stirred for 3 hours at RT. 500 ml of a saturated solution of ammonium chloride are added and the solvents are concentrated under vacuum. The aqueous phase is extracted with AcOEt, the organic phase is washed with a saturated solution of NaCl and with water and dried over sodium sulfate and the solvent is evaporated off under vacuum to give 5.6 g of the expected product after crystallization from a THF/AcOEt mixture. M.p.=204°-205° C.

1. temperatureis cooled to +4° C.
2. concentrationthe solvents are concentrated under vacuum
3. extractionThe aqueous phase is extracted with AcOEt
4. washthe organic phase is washed with a saturated solution of NaCl and with water
5. dry with materialdried over sodium sulfate
6. customthe solvent is evaporated off under vacuum