反应详情

A solution of 11.3 g (49.6 mmol) of a mixture that consists of 4-nitro-thiophene-2-sulfonyl chloride and 5-nitro-thiophene-2-sulfonyl chloride (ratio: 1.4/1.0) in acetone is added while being stirred to a saturated solution of ammonia in 170 ml of acetone at −35° C. After 30 minutes, the batch is filtered and concentrated by evaporation. The crude product is dissolved without further purification in 100 ml of ethanol. It is mixed with 6 g of Raney nickel and hydrogenated for 8 hours under low pressure at room temperature. The batch is filtered and concentrated by evaporation. 11.7 g of a mixture that consists of 4-amino-thiophene-2-sulfonic acid amide and 5-amino-thiophene-2-sulfonic acid amide is obtained at a ratio of 2:1, which is used without further purification.

1. additionis added
2. filtrationthe batch is filtered
3. concentrationconcentrated by evaporation
4. dissolutionThe crude product is dissolved without further purification in 100 ml of ethanol
5. additionIt is mixed with 6 g of Raney nickel
6. waithydrogenated for 8 hours under low pressure at room temperature
7. filtrationThe batch is filtered
8. concentrationconcentrated by evaporation