HRID1697201

反应详情

EQUATION

反应方程式

HRID 1697201 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

3-(Methoxymethoxy)-6-neopentylpicolinonitrile (8.3 g, 35 mmol) was dissolved in THF (125 mL). The solution was cooled to 0° C. and methylmagnesium chloride (24 ml, 71 mmol) (3.0 M in Et2O) was added. The reaction mixture stirred for 2 h at rt under N2 then quenched with saturated NH4Cl (50 mL) and extracted with EtOAc (3×50 mL). The organic layer was dried over MgSO4 and evaporated to give the crude product as a yellow oil. Purification of the crude residue by ISCO (40 g SiO2, O-40% EtOAc/Hexane) gave 1-(3-(methoxymethoxy)-6-neopentylpyridin-2-yl)ethanone (3.8 g, 43% yield) as a clear, light orange oil.

WORKUP

后处理

  1. customthen quenched with saturated NH4Cl (50 mL)
  2. extractionextracted with EtOAc (3×50 mL)
  3. dry with materialThe organic layer was dried over MgSO4
  4. customevaporated
  5. customto give the crude product as a yellow oil
  6. customPurification of the crude residue by ISCO (40 g SiO2