HRID1435980

反应详情

EQUATION

反应方程式

HRID 1435980 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Glacial acetic acid (2 ml) and 6M hydrochloric acid (4.25 ml) were added to the 3-(1-benzoylaminoisoquinolin-6ylsulfanyl)piperidine-1-carboxylic acid tert-butyl ester (18 mg, 0.039 mmol) and the mixture was refluxed for 24 h. The mixture was then concentrated in vacuo to give a residue. The residue was loaded onto a pre-acidified SCX column using methanol and then eluted with 2M ammonia in methanol to give 6-(piperidin-3-ylsulfanyl)isoquinolin-1--ylamine which was further purified using prep-HPLC, EIMS: m/z=260.3 [M+H]+

WORKUP

后处理

  1. temperaturethe mixture was refluxed for 24 h
  2. concentrationThe mixture was then concentrated in vacuo
  3. customto give a residue
  4. washeluted with 2M ammonia in methanol