HRID1394598

反应详情

EQUATION

反应方程式

HRID 1394598 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

A slurry of 365 mg (0.859 mmol) of 2-acetyl-4-(2-methoxymethoxy-3,5-di-tert-butylphenyl)benzo[b]thiophene into a mixture of 5 mL of THF and 5 mL of aqueous 6N HCl was heated to 50° C. overnight. After cooling, the THF was evaporated and the aqueous solution was extracted with ethyl acetate. The organic layer was dried over MgSO4 and evaporated under reduced pressure. The crude 2-acetyl-4-(2-hydroxy-3,5-di-tert-butylphenyl)benzo[b]thiophene was directly used in the next step. 1H-NMR (CDCl3), δ: 7.92 (d, J=8.0 Hz, 1H), 7.73 (s, 1H), 7.58 (t, J=7.4 Hz, 1H), 7.47 (d, J=2.6 Hz, 1H), 7.42 (d, J=2.3 Hz, 1H), 7.14 (d, J=2.4 Hz, 1H), 5.03 (s, 1H), 2.57 (s, 3H), 1.48 (s, 9H), 1.34 (s, 9H).

WORKUP

后处理

  1. temperatureAfter cooling
  2. customthe THF was evaporated
  3. extractionthe aqueous solution was extracted with ethyl acetate
  4. dry with materialThe organic layer was dried over MgSO4
  5. customevaporated under reduced pressure