HRID487699

反应详情

EQUATION

反应方程式

HRID 487699 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

To a cooled solution of 2-(5-methoxybenzofuran-2-yl)-4,5,6,7-tetrahydro-8H-thiazolo[5,4-b]azepine (1.3 g) and pyridine (0.65 ml) in N,N-dimethylformamide (20 ml), a solution of acetyl chloride (0.41 g) in dichloromethane (2 ml) was added dropwise below 10° C. After being stirred for 2 hours, the resulting mixture was poured into brine and extracted with ethyl acetate. The organic layer was washed with brine, dried over magnesium sulfate and concentrated under reduced pressure to give a syrup, which was crystallized from ethanol and collected by filtration to give 8-acetyl-2-(5-methoxybenzofuran-2-yl) 4,5,6,7-tetrahydro-8H-thiazolo[5,4-b]azepine (1.07 g).

WORKUP

后处理

  1. extractionextracted with ethyl acetate
  2. washThe organic layer was washed with brine
  3. dry with materialdried over magnesium sulfate
  4. concentrationconcentrated under reduced pressure
  5. customto give a syrup, which
  6. customwas crystallized from ethanol
  7. filtrationcollected by filtration