HRID1024041

反应详情

EQUATION

反应方程式

HRID 1024041 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

A mixture of 109b (4.3 g, 19.5 mmol) in formic acid (10 mL) was heated at 80° C. for 1 h. After cooled to room temperature, the reaction mixture was poured into aqueous Na2CO3 (30 mL) and the mixture was extracted with ethyl acetate (30 mL×3). The combined organic phase was dried over anhydrous Na2SO4, filtered, and evaporated under reduced pressure to afford 109c as a brown solid (3.5 g, 77%). LCMS: [M+H]+ 233. 1H NMR (500 MHz, CDCl3) δ 10.05 (bs, 1H), 8.18 (s, 1H), 7.64 (bs, 1H), 7.50 (s, 1H).

WORKUP

后处理

  1. temperatureAfter cooled to room temperature
  2. extractionthe mixture was extracted with ethyl acetate (30 mL×3)
  3. dry with materialThe combined organic phase was dried over anhydrous Na2SO4
  4. filtrationfiltered
  5. customevaporated under reduced pressure