反应详情

温度

80 °C

To 6-bromo-thianthrene-2-carboxylic acid (9 g, 28 mmol) in methanol (180 ml) was slowly added conc. H2SO4 (5 ml). The milky white suspension was heated to 80° C. until all the solid had gone into solution (2 hrs). The suspension was concentrated in vacuo. Water (100 ml) was added and the organics were then extracted with dichloromethane (3×70 ml), dried over MgSO4 and evaporated in vacuo, yielding to a yellow solid. (4.48 g, 45%). 1HNMR (300 MHz, CDCl3): δH=3.94 (3H, s); 7.13 (1H, t), 7.44 (1H, dd), 7.54 (1H, dd) 7.61 (1H, d), 7.93 (1H, dd), 8.13 (1H, d).

1. customhad gone into solution (2 hrs)
2. concentrationThe suspension was concentrated in vacuo
3. additionWater (100 ml) was added
4. extractionthe organics were then extracted with dichloromethane (3×70 ml)
5. dry with materialdried over MgSO4
6. customevaporated in vacuo
7. customyielding to a yellow solid