HRID1633645
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
PROCEDURE
实验过程
1.5 g (0.4 mmol) crude 5-(5-Methanesulfonyloxy-pentyl)-indole-1-carboxylic acid tert-butyl ester in 3 ml DMF were treated with 1.15 ml (12 mmol) N-allylmethylamine at 60° C. for 1 h. The solution was concentrated in vacuo and, the residue was dissolved in water and ether, 0.5M NaOH was added and the inorganic phase was extacted with ether. The combined organic phases were washed with water and dried over Na2SO4. Column chromatography on silica gel yielded 1.35 g (94%) 5-[5-(Allyl-methyl-amino)-pentyl]-indole-1-carboxylic acid tert-butyl ester as light yellow oil, MS: 357 (MH+).
WORKUP
后处理
- concentrationThe solution was concentrated in vacuo
- dissolutionthe residue was dissolved in water
- additionether, 0.5M NaOH was added
- washThe combined organic phases were washed with water
- dry with materialdried over Na2SO4