HRID408584
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
CONDITIONS
反应条件
- 温度
- 20 °C
PROCEDURE
实验过程
To a suspension of K2CO3 (1.5 eq.) and (R)-1-(4-chloro-phenyl)-ethylamine (0.9 eq.) in MeCN was added 4-bromo-butyric acid methyl ester (1 eq.) and KI (0.1 eq.). The reaction was stirred for 15 h at 20° C., then heated to reflux until completion. The crude was partitioned between water and EtOAc. The organic layer was washed with brine, dried over MgSO4, filtered and concentrated under reduced pressure. The crude was purified by chromatography on silica gel (elution with DCM/MeOH: 99/1 to 90/10) to afford 4-[(R)-1-(4-chloro-phenyl)-ethylamino]-butyric acid methyl ester.
WORKUP
后处理
- temperatureheated
- temperatureto reflux until completion
- customThe crude was partitioned between water and EtOAc
- washThe organic layer was washed with brine
- dry with materialdried over MgSO4
- filtrationfiltered
- concentrationconcentrated under reduced pressure
- customThe crude was purified by chromatography on silica gel (elution with DCM/MeOH: 99/1 to 90/10)