HRID2403465
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 suspension of NaH (24 mg, 0.6 mmol 1.2 equiv) in anhydrous THF, HLA20 (140 mg, 0.5 mmol, 1.0 equiv) was added under Ar at 0° C. The resulting mixture was stirred for 20 min at 0° C. A solution of dimethyl carbamoyl chloride (1.1 equiv) in anhydrous THF was added, and the stirring was continued for 24 h at room temperature. After evaporation of the solvent, water was added and the resulting mixture was extracted with ethyl acetate. The combined organic extracts were washed with brine and dried with NaSO4. Evaporation of the solvent gave a crude product that was purified by RP HPLC.
WORKUP
后处理
- additionwas added under Ar at 0° C
- waitthe stirring was continued for 24 h at room temperature
- customAfter evaporation of the solvent, water
- additionwas added
- extractionthe resulting mixture was extracted with ethyl acetate
- washThe combined organic extracts were washed with brine
- dry with materialdried with NaSO4
- customEvaporation of the solvent