HRID1594
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
To a solution of 2-methoxycarbonyl-(1RS,4aSR,8aSR)-perhydoisoquinoline-1-carboxylic acid t-butyl ester (81.2 g, 273 mmol) in EtOH (500 mL) was added sodium ethoxide (21% in ethanol) (88.4 mL, 273 mmol) and the reaction mixture was refluxed (24 h). The organic solvent was evaporated in vacuo, ethyl acetate (400 mL) and water (100 mL) was added to the residue. The organic layer was separated, washed twice with water, dried (MgSO4), filtered, and the filtrate was concentrated in vacuo to afford an oil of pure title compound (70 g,0.95%); FAB-MS 270 (MH+); TLC Rf (A) 0.61.
WORKUP
后处理
- temperaturethe reaction mixture was refluxed (24 h)
- customThe organic solvent was evaporated in vacuo, ethyl acetate (400 mL) and water (100 mL)
- additionwas added to the residue
- customThe organic layer was separated
- washwashed twice with water
- dry with materialdried (MgSO4)
- filtrationfiltered
- concentrationthe filtrate was concentrated in vacuo