HRID1466541
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
- 0 °C
PROCEDURE
实验过程
To a solution of di-tert-butyl (4S)-4-(3-hydroxypropyl)-N-trityl-L-glutamate (203.4 mg, 0.36 mmol) and triethylamine (150 μL, 1.09 mmol) in dichloromethane (5.0 mL) was added quinoline-8-sulfonyl chloride (124.1 mg, 0.55 mmol) at 0° C. The reaction mixture was stirred at 0° C. for 3 h and at room temperature for overnight and then water was added. The organic layer was separated, and aqueous layer was extracted with dichloromethane. Combined organic solution was dried over sodium sulfate, and concentrated in vacuo. The residue was purified by flash column chromatography (MeOH/CH2Cl2=1/99) to give the desired product (140 mg, 51%) as a white solid.
WORKUP
后处理
- customThe organic layer was separated
- extractionaqueous layer was extracted with dichloromethane
- dry with materialCombined organic solution was dried over sodium sulfate
- concentrationconcentrated in vacuo
- customThe residue was purified by flash column chromatography (MeOH/CH2Cl2=1/99)