HRID275857
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 tetrahydrofuran (30 ml) solution of N-methyl-N-methyloxy-2-aminobenzamide (2.70 g) and N-tert-butoxycarbonyl-3-bromobenzylamine (2.86 g) was cooled to −78° C. To the solution was gradually added dropwise a hexane solution of n-butyl lithium (1.6 mol/L) (31 ml). To the mixture were then added water (70 ml) and acetic acid ethyl ester (70 ml). The organic layer was washed with water and dried over anhydrous MgSO4. The solvent was then distilled off. The residual oily compound was purified by means of a silica gel column chromatography to give 2-amino-3′-(tert-butoxycarbonylaminomethyl)benzophenone as a yellow oily product (1.2 g).
WORKUP
后处理
- washThe organic layer was washed with water
- dry with materialdried over anhydrous MgSO4
- distillationThe solvent was then distilled off
- customThe residual oily compound was purified by means of a silica gel column chromatography