HRID1019769

反应详情

EQUATION

反应方程式

HRID 1019769 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A 2M solution of LiBH4 in THF (2 mmol) was added drop-wise to a stirred solution of methyl 2-chloro-5-methoxy-4-nitrobenzoate (1 mmol) in dry THF (10 mL) at 0° C. The mixture was allowed to warm to room temperature and stirred for 5 hours. EtOAc (10 mL) was added to the mixture followed by saturated NH4Cl solution (2 mL) and stirring continued for 15 minutes. The mixture was partitioned between EtOAc (10 mL) and water (10 mL) and the separated aqueous phase was extracted with EtOAc (10 mL). The combined organic extracts were dried (Na2SO4) and concentrated under reduced pressure to afford the title compound (89%) which was used without further purification.

WORKUP

后处理

  1. stirringstirring
  2. waitcontinued for 15 minutes
  3. customThe mixture was partitioned between EtOAc (10 mL) and water (10 mL)
  4. extractionthe separated aqueous phase was extracted with EtOAc (10 mL)
  5. dry with materialThe combined organic extracts were dried (Na2SO4)
  6. concentrationconcentrated under reduced pressure