HRID1451657

反应详情

EQUATION

反应方程式

HRID 1451657 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 1-(2-bromoethyl)-4-nitrobenzene (3.7 g), 1,2,3,4-tetrahydro-7-methoxyisoquinoline (2.7 g; Daniel J. Sall and Gary L. Grunewald, J. Med. Chem. 1987, 30, 2208-2216) and potassium carbonate (6.7 g) in isopropanol (150 ml) was stirred under reflux for 48 h. The mixture was evaporated to dryness, and the residue was extracted with dichloromethane. The organic layer was washed with water, dried, filtered and evaporated. The residue was then purified by column chromatography elating with dichloromethane/methanol (99:1) to give the title compound (1.6 g) as an orange solid, MP: 92°-94°. NMR includes signals at d 3.6 (2H,m,N--CH2Ar), 3.7 (3H,s,OCH3).

WORKUP

后处理

  1. temperatureunder reflux for 48 h
  2. customThe mixture was evaporated to dryness
  3. extractionthe residue was extracted with dichloromethane
  4. washThe organic layer was washed with water
  5. customdried
  6. filtrationfiltered
  7. customevaporated
  8. customThe residue was then purified by column chromatography