反应详情

The compound from step (a) above (24.2 mmol), N,N-dimethylaminothiocarbamoyl chloride (37 mmol) in dimethyl formamide (250 ml) were stirred rapidly in the presence of potassium carbonate (60 mmol) for 24 hours, adding more potassium carbonate (1 g) after 18 hours. The mixture was acidified (to pH4) with dilute hydrochloric acid and extracted with ethyl acetate (3 times). The combined extracts were washed with water (4 times), dried (anhydrous sodium sulphate) and evaporated to yield a brown solid, which was triturated with ether, and filtered to give the sub-title compound.

1. extractionextracted with ethyl acetate (3 times)
2. washThe combined extracts were washed with water (4 times)
3. dry with materialdried (anhydrous sodium sulphate)
4. customevaporated
5. customto yield a brown solid, which
6. customwas triturated with ether
7. filtrationfiltered