HRID2261322

反应详情

EQUATION

反应方程式

HRID 2261322 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2.20 g of [5-(1H-pyrrol-1-yl)-1-t-butyl-1H-pyrazol-4-yl]methanol was dissolved in 20 ml of dichloromethane, and 0.73 ml of thionyl chloride was added. The mixture was stirred at room temperature for 1.5 hours and then concentrated under reduced pressure. After aqueous saturated sodium hydrogen carbonate was added, the residue was extracted with ethyl acetate. The organic layer was dried over anhydrous magnesium sulfate, filtered and then concentrated under reduced pressure. The residue was subjected to silica gel column chromatography to obtain 2.35 g of 4-(chloromethyl)-5-(1H-pyrrol-1-yl)-1-t-butyl-1H-pyrazole.

WORKUP

后处理

  1. concentrationconcentrated under reduced pressure
  2. additionAfter aqueous saturated sodium hydrogen carbonate was added
  3. extractionthe residue was extracted with ethyl acetate
  4. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated under reduced pressure