HRID1097365
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
2-fluorobenzylbromide (0.369 g) was added portionwise to a solution of the product of example 32 step b) (0.5 g) and diisopropylethylamine (0.26 g) in DMSO/N-methylpyrrolidinone (4 ml/0.5 ml) at 50° C. and stirring maintained for 1 h. The mixture was partitioned between H2O (200 ml) and EtOAc (120 ml). The organics were recovered and washed further with H2O (200 ml), dried over MgSO4 and concentrated onto silica gel. The subtitle compound was purified by flash chromatography using DCM then EtOAc as eluents to yield a white solid (245 mg, 35%).
WORKUP
后处理
- temperaturemaintained for 1 h
- customThe mixture was partitioned between H2O (200 ml) and EtOAc (120 ml)
- customThe organics were recovered
- washwashed further with H2O (200 ml)
- dry with materialdried over MgSO4
- concentrationconcentrated onto silica gel
- customThe subtitle compound was purified by flash chromatography