Реакция #62063

Уравнение реакции

6-bromo-thianthrene-2-carboxylic acid

H2SO4

methanol

→

6-Bromo-thianthrene-2-carboxylic acid methyl ester

Условия реакции

Обработка

1. 1
   Другоеhad gone into solution (2 hrs)
2. 2
   КонцентрированиеThe suspension was concentrated in vacuo
3. 3
   workup.ADDITIONWater (100 ml) was added
4. 4
   Экстракцияthe organics were then extracted with dichloromethane (3×70 ml)
5. 5
   Сушкаdried over MgSO4
6. 6
   Другоеevaporated in vacuo
7. 7
   Другоеyielding to a yellow solid

Методика

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).

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