反应详情

温度

120 °C

A mixture of N,N-dimethyl-N'-(6-oxido-thieno[2,3-c]pyridine-2-sulfonyl)formamidine (3.5 g, 12.3 mmol) in acetic anhydride (20 ml), under a nitrogen atmosphere, was heated at 120° C. for 3 hours. The dark solution was poured into ice/water and stirred for 1/2 hour. The product was extracted into methylene chloride, washed with sodium carbonate solution, dried over anhydrous sodium sulfate and evaporated to give 4.77 g of crude product. This residue was triturated with methylene chloride/diethyl ether to give 2.0 g (50% yield) of pure product. Recrystallization from ethyl acetate gave product with a broad melting point of 184°-191° C.

1. extractionThe product was extracted into methylene chloride
2. washwashed with sodium carbonate solution
3. dry with materialdried over anhydrous sodium sulfate
4. customevaporated
5. customto give 4.77 g of crude product
6. customThis residue was triturated with methylene chloride/diethyl ether