反应详情

To a solution of 1.04 g of 3-(5-fluorobenzothiazol-2-ylmethoxy)benzyl alcohol (Preparation L) in 60 ml of dry tetrahydrofuran was added 2.38 g of carbontetrabromide and 1.89 g of triphenylphosphine and the reaction stirred under nitrogen at room temperature for 1.5 hours. The reaction mixture was filtered, treated with 100 ml of water and extracted with ethyl acetate. The extracts were washed with water and a brine solution and dried over sodium sulfate. The solvent was removed and the residual brown solid chromatographed on 200 g of silica gel using from 5-10% ethyl acetate--95-90% hexane (v:v). The fractions containing the product were combined and concentrated to give 910 mg of the titled product, m.p. 99°-100° C.

1. filtrationThe reaction mixture was filtered
2. additiontreated with 100 ml of water
3. extractionextracted with ethyl acetate
4. washThe extracts were washed with water
5. dry with materiala brine solution and dried over sodium sulfate
6. customThe solvent was removed
7. customthe residual brown solid chromatographed on 200 g of silica gel using from 5-10% ethyl acetate--95-90% hexane (v:v)
8. additionThe fractions containing the product
9. concentrationconcentrated