反应详情

5-Methoxycarbonylthieno[2,3-b]thiophene-2-sulfonamide (0.83 g., 3 mmoles) and 2,3-dihydroxypropylamine (1.37 g., 15 mmoles) were dissolved in hot methanol and refluxed for 48 hours. The reaction was worked up by evaporating the methanol in vacuo. Water (7 mL) was added followed by the dropwise addition of conc. HCl until strongly acidic (~1.8 pH). The product crystallized out and was collected, washed with water and dried to give 0.90 g of crude product. Recrystallization from nitromethane gave 0.73 g of 5-(N-2,3-dihydroxypropylcarbamoyl)thieno[2,3-b]thiophene-2-sulfonamide, m.p. 117°-118° C.

1. temperaturerefluxed for 48 hours
2. customby evaporating the methanol in vacuo
3. additionWater (7 mL) was added
4. additionfollowed by the dropwise addition of conc. HCl until strongly acidic (~1.8 pH)
5. customThe product crystallized out
6. customwas collected
7. washwashed with water
8. customdried
9. customto give 0.90 g of crude product
10. customRecrystallization from nitromethane