HRID906467
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
A solution of tert-Butyl (3R)-3-{[(2-{[1-({[tert-butyl(dimethyl)silyl]oxy}methyl)-cyclopropyl]methyl}-6-[5-(cyclopropylcarbamoyl)-3-fluoro-2-methylphenyl]-1-oxo-1,2-dihydroisoquinolin-4-yl)sulfanyl]methyl}piperidine-1-carboxylate (Example 63e, 110 mg) in 4N HCl in dioxane (1 mL) and ethanol (3 mL) was stirred for 20 h before being concentrated in vacuo. The residue was dissolved in methanol (2 mL) and loaded onto a 10 g SCX cartridge. The impurities were washed through with methanol (50 mL) and discarded. The product was eluted with 1N methanolic ammonia (50 mL) and evaporated in vacuo to afford the title product (63 mg) as a white solid.
WORKUP
后处理
- concentrationbefore being concentrated in vacuo
- dissolutionThe residue was dissolved in methanol (2 mL)
- washThe impurities were washed through with methanol (50 mL)
- washThe product was eluted with 1N methanolic ammonia (50 mL)
- customevaporated in vacuo