HRID1454316

反应详情

EQUATION

反应方程式

HRID 1454316 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a cold solution (−20° C.) of 3.3 g (20 mmol) 7-methoxy-benzofuranone in 30 mL methylene chloride was added 8.3 mL (6.0 mmol) of triethylamine. To the cold mixture, a solution of 8.5 g (30 mmol) of triflic anhydride in 20 ml of methylene chloride was added dropwise. The temperature was kept at −20° C. or 1 hour. The reaction was then quenched with 100 mL of saturated aqueous sodium bicarbonate aand extracted with methylene chloride (2×150 mL). The combined organic extracts were dried over magnesium sulfate and concentrated in vacuum to give 5.6 g of the desired product. MS (ES) m/z (relative intensity): 265 (M+H,100);

WORKUP

后处理

  1. customThe reaction was then quenched with 100 mL of saturated aqueous sodium bicarbonate
  2. extractionextracted with methylene chloride (2×150 mL)
  3. dry with materialThe combined organic extracts were dried over magnesium sulfate
  4. concentrationconcentrated in vacuum