反应详情

A suspension of 18.15 g of 5-chloroisatin in 45 ml of THF is cooled to +4° C., 200 ml of a 2M solution of cyclohexylmagnesium chloride in ether are added dropwise and the mixture is stirred for 3 hours at RT. 900 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 dried over sodium sulfate and the solvent is evaporated off under vacuum to give 4 g of the expected product after crystallization from a THF/AcOEt mixture.

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
5. dry with materialdried over sodium sulfate
6. customthe solvent is evaporated off under vacuum