HRID2261321

反应详情

EQUATION

反应方程式

HRID 2261321 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1.30 g of lithium aluminum hydride was suspended in 50 ml of tetrahydrofuran and thereto, under a nitrogen atmosphere, a solution of 8.95 g of ethyl 5-(1H-pyrrol-1-yl)-1-t-butyl-1H-pyrazole-4-carboxylate in 20 ml of tetrahydrofuran was added dropwise over 15 minutes under ice-cooling. The mixture was stirred for 8 hours under ice-cooling. After water was added, the reaction mixture 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 7.06 g of [5-(1H-pyrrol-1-yl)-1-t-butyl-1H-pyrazol-4-yl]methanol.

WORKUP

后处理

  1. temperaturecooling
  2. temperaturecooling
  3. extractionthe reaction mixture was extracted with ethyl acetate
  4. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated under reduced pressure