HRID1644555

反应详情

EQUATION

反应方程式

HRID 1644555 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 0.45 g of 6-chloro-1-methylthio-4-(4-nitrophenyl)-3,4-dihydroisoquinoline and 30 ml of ammonia-saturated THF solution was heated in an autoclave at 80° C. for 10 hours and then at 12° C. for a further 15 hours. Subsequent MPLC on an MPRC cartridge and a mixture of 20 parts by volume of ethyl acetate:10 parts by volume of n-heptane:3 parts by volume of glacial acetic acid leads to elution of starting material (6-chloro-1-methylthio-4-(4-nitrophenyl)-3,4-dihydroisoquinoline). Subsequent elution with methanol results in 1-amino-6-chloro-4-(4-nitrophenyl)-3,4-dihydroisoquinoline.

WORKUP

后处理

  1. wash10 parts by volume of n-heptane:3 parts by volume of glacial acetic acid leads to elution of starting material (6-chloro-1-methylthio-4-(4-nitrophenyl)-3,4-dihydroisoquinoline)
  2. washSubsequent elution with methanol
  3. customresults in 1-amino-6-chloro-4-(4-nitrophenyl)-3,4-dihydroisoquinoline