HRID22409

反应详情

EQUATION

反应方程式

HRID 22409 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

To a solution of 2-amino-N-[2-(2-fluorobenzoyl)-1H-pyrrol-1-yl]acetamide hydrobromide hemihydrate (2.09 g) in 10 ml of anhydrous dimethylformamide and 40 ml of anhydrous DCM were added pyridine (1.89 g) and acetic anhydride (1.22 g). The reaction mixture was stirred at room temperature for 1 hour, subsequently diluted with water and extracted with DCM. The combined organic layers were washed with 5% hydrochloric acid and water, dried over magnesium sulfate and evaporated in vacuo. The residual oil was recrystallized from DCM/ethyl ether affording the product as crystals (1.58 g), m.p. 146°-147° C.

WORKUP

后处理

  1. extractionextracted with DCM
  2. washThe combined organic layers were washed with 5% hydrochloric acid and water
  3. dry with materialdried over magnesium sulfate
  4. customevaporated in vacuo
  5. customThe residual oil was recrystallized from DCM/ethyl ether affording the product as crystals (1.58 g), m.p. 146°-147° C.