HRID2401198

反应详情

EQUATION

反应方程式

HRID 2401198 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. customThe reaction was quenched with water (25 mL)
  2. stirringwith stirring
  3. extractionextracted with ethyl acetate (50 mL)
  4. dry with materialThe combined organic layers were dried (MgSO4)
  5. filtrationfiltered
  6. customevaporated to dryness
  7. customto afford the crude residues
  8. customCrude residues were then purified on Biotage Isolera on a pre-packed silica cartaridge (25 g)
  9. washeluting with 0-20% ethyl acetate-isohexane
  10. customevaporated in vacuo