反应详情

To a solution of the compound obtained in Step A (87 mmoles) and AlCl3 in a DCM/nitromethane mixture (80 ml/80 ml) there is added, dropwise, at −30° C., dichloro-methoxy-methane (130.5 mmoles). After stirring for two hours, the reaction mixture is poured into 800 ml of ice-cold water. The aqueous phase is extracted with AcOEt, and then the organic phases are combined. The organic phase is washed with saturated aqueous NaCl solution, dried over sodium sulphate, filtered and evaporated to dryness to yield the title product (brown crystals), which is used directly in the next Step.

1. customat −30° C.
2. extractionThe aqueous phase is extracted with AcOEt
3. washThe organic phase is washed with saturated aqueous NaCl solution
4. dry with materialdried over sodium sulphate
5. filtrationfiltered
6. customevaporated to dryness