反应详情

A solution of 7-bromo-4-chlorothieno[3,2-d]pyrimidine (see below for preparation) (2.0 g), sodium hydrosulfide hydrate (0.66 g) and N-methylpyrrolidinone (10 ml) was heated at 102° C. for 1 hour. Water (500 ml) and ethyl acetate (500 ml) were added and stirred for 1 hour. The layers were separated and the aqueous phase extracted with ethyl acetate (300 ml). The combined organic extracts were washed with brine (300 ml), dried (MgSO4), treated with activated charcoal, then filtered through a silica pad and the solvent removed to give the title product, m.p. 328° C.

1. customThe layers were separated
2. extractionthe aqueous phase extracted with ethyl acetate (300 ml)
3. washThe combined organic extracts were washed with brine (300 ml)
4. dry with materialdried (MgSO4)
5. additiontreated with activated charcoal
6. filtrationfiltered through a silica pad
7. customthe solvent removed