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 stirred solution of 1-(6-chloro-4-pyrimidinyl)ethanone (Intermediate 18, 500 mg, 3.19 mmol)) in THF (5 mL) was added methylmagnesium bromide (1.171 mL, 3.51 mmol), and the resulting mixture stirred under argon at 0° C. for 2 hrs. The reaction was quenched with water (25 mL) with stirring and extracted with ethyl acetate (50 mL). The combined organic layers were dried (MgSO4), filtered and evaporated to dryness to afford the crude residues. Crude residues were then purified on Biotage Isolera on a pre-packed silica cartaridge (25 g) eluting with 0-20% ethyl acetate-isohexane. The appropriate fractions were combined and evaporated in vacuo to give the required product as a yellow oil (218 mg).
WORKUP
后处理
- customThe reaction was quenched with water (25 mL)
- stirringwith stirring
- extractionextracted with ethyl acetate (50 mL)
- dry with materialThe combined organic layers were dried (MgSO4)
- filtrationfiltered
- customevaporated to dryness
- customto afford the crude residues
- customCrude residues were then purified on Biotage Isolera on a pre-packed silica cartaridge (25 g)
- washeluting with 0-20% ethyl acetate-isohexane
- customevaporated in vacuo