HRID394457

反应详情

EQUATION

反应方程式

HRID 394457 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
40 °C

PROCEDURE

实验过程

1.2 g (4.4 mmol) of 7-(morpholin-4-ylsulfonyl)-1,2,3,4-tetra-hydroisoquinoline and 1.0 g (10 mmol) of triethylamine were dissolved in DMF at 40° C., 1.1 g (6.6 mmol) of 1-bromo-3-chloropropane were added dropwise, and the mixture was stirred at 40° C. for 3 h. For workup, the mixture was concentrated, and the residue was taken up in water and extracted with methyl tert-butyl ether. Drying over sodium sulfate, filtration and removal of the solvent were followed by purification by chromatography (silica gel; mobile phase: methylene chloride with 2% methanol) to afford 0.7 g (2 mmol) of a pale oil.

WORKUP

后处理

  1. concentrationFor workup, the mixture was concentrated
  2. extractionextracted with methyl tert-butyl ether
  3. dry with materialDrying over sodium sulfate, filtration and removal of the solvent
  4. customwere followed by purification by chromatography (silica gel; mobile phase: methylene chloride with 2% methanol)