反应详情

Chlorosulfonic acid (3.05 ml, 45.9 mmole) from the above Step was added to a suspension of anhydrous sodium sulfate (0.71 g) in methylene chloride (30 ml). After stirring for 25 minutes at room temperature, (5-nitro-indol-1-yl)-acetonitrile (1.00 g) dissolved in methylene chloride was added via syringe. After stirring for 2 h, the reaction mixture was worked up by the cautious addition of ice. When the ice had melted, the mixture was filtered to afford an off-white powder which was washed well with water to afford 0.806 g of 1-carbamoylmethyl-5-nitro-1H-indole-3-sulfonyl chloride (51% yield).

1. additionwas added via syringe
2. stirringAfter stirring for 2 h
3. additionthe reaction mixture was worked up by the cautious addition of ice
4. filtrationthe mixture was filtered
5. customto afford an off-white powder which
6. washwas washed well with water