HRID2682

反应详情

EQUATION

反应方程式

HRID 2682 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

7-Hydroxy-4-methylcoumarin-3-acetic acid (1) (1 gm, 4.3 mmol) was suspended in anhydrous ethanol (15 mL), concentrated sulfuric acid (1.5 mL) was added and the mixture was heated at reflux for 1 hour. The reaction mixture was cooled to room temperature, diluted with ethyl acetate (100 mL), washed with 5% NaHCO3 (5×50 mL), water (2×50 mL), saturated NaCl (2×50 mL) dried with sodium sulfate, filtered and the filtrate was evaporated under reduced pressure to give 1.04 gm (4.0 mmol, 92% yield of 2 as a white solid.

WORKUP

后处理

  1. temperaturethe mixture was heated
  2. temperatureat reflux for 1 hour
  3. washwashed with 5% NaHCO3 (5×50 mL), water (2×50 mL), saturated NaCl (2×50 mL)
  4. dry with materialdried with sodium sulfate
  5. filtrationfiltered
  6. customthe filtrate was evaporated under reduced pressure