HRID1435980
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperaturethe mixture was refluxed for 24 h
- concentrationThe mixture was then concentrated in vacuo
- customto give a residue
- washeluted with 2M ammonia in methanol