反应详情

A solution of 0.2 mol of ethyl magnesium bromide in diethyl ether was added to a solution of 22.0 g (0.1 mol) of 2,4-dichloro-6-fluorobenzothiazole and 3.3 g (5 mmol) of dichlorobis(triphenylphosphine)nickel in 0.5 1 of diethyl ether. Stirring was carried out for 2 hours, after which the mixture was poured onto saturated aqueous ammonium chloride solution. The product was extracted with diethyl ether. The combined organic phases were washed with water, dried over magnesium sulfate and finally evaporated down. Purification of the crude product was effected by means of silica gel chromatography (eluent: 8:2 cyclohexane/methyl tert-butyl ether). Yield: 10.3 g.

1. extractionThe product was extracted with diethyl ether
2. washThe combined organic phases were washed with water
3. dry with materialdried over magnesium sulfate
4. customfinally evaporated down
5. customPurification of the crude product