HRID547747

反应详情

EQUATION

反应方程式

HRID 547747 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 8.65 g (19.6 mmol) (6-chloro-4-iodo-pyridin-3-yl)-methyl-carbamic acid tert-butyl ester in 20 ml dichloromethane were added 20.0 ml (261 mmol) trifluoroacetic acid at 0° C. After stirring for 2 h at room temperature the reaction mixture was concentrated in vacuo. The residue was treated with 50 ml saturated sodium carbonate solution and extracted three times with 75 ml ethyl acetate. The combined organic layers were washed with 50 ml brine, dried over sodium sulfate and concentrated in vacuo to give 6.1 g (87%) of the title compound as a light brown solid.

WORKUP

后处理

  1. concentrationwas concentrated in vacuo
  2. additionThe residue was treated with 50 ml saturated sodium carbonate solution
  3. extractionextracted three times with 75 ml ethyl acetate
  4. washThe combined organic layers were washed with 50 ml brine
  5. dry with materialdried over sodium sulfate
  6. concentrationconcentrated in vacuo