HRID2246615

反应详情

EQUATION

反应方程式

HRID 2246615 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of ((4-bromo-2-fluorophenyl)(tetrahydro-3-furanyl)methanone (Intermediate 7, 850 mg) 1,1-dimethylethyl hydrazinecarboxylate (616 mg) and acetic acid (1 mL) in methanol (5 mL) was stirred at reflux under nitrogen for 20 h. The solvent was removed under vacuum and the residue was partitioned between ethyl acetate and water. The organic phase was washed with sodium bicarbonate (1M, 10 mL), dried using a hydrophobic filter tube and concentrated under vacuum to give the title compound as a brown oil (1.1 g).

WORKUP

后处理

  1. temperatureat reflux under nitrogen for 20 h
  2. customThe solvent was removed under vacuum
  3. customthe residue was partitioned between ethyl acetate and water
  4. washThe organic phase was washed with sodium bicarbonate (1M, 10 mL)
  5. customdried
  6. concentrationconcentrated under vacuum