HRID549240

反应详情

EQUATION

反应方程式

HRID 549240 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Potassium acetate (3.93 g, 40.0 mmol) and bromine (3.58 g, 22.4 mmol) were sequentially added to a solution of 1-propyl-5-(tetrahydro-2H-pyran-4-ylmethyl)-1H-pyrazole-3-carbonitrile (3.98 g, 16 mmol) in acetic acid (32 mL). The reaction was stirred for 40 hours at room temperature. Saturated aqueous sodium hydrogensulfite was added until the reaction became colorless. Most of the acetic acid was removed under reduced pressure, and 2M aqueous sodium carbonate was added. A precipitate formed, was isolated by filtration, washed with water, and dried on the vacuum filter funnel to provide 4.91 g of 4-bromo-1-propyl-5-(tetrahydro-2H-pyran-4-ylmethyl)-1H-pyrazole-3-carbonitrile as a white solid.

WORKUP

后处理

  1. customMost of the acetic acid was removed under reduced pressure, and 2M aqueous sodium carbonate
  2. additionwas added
  3. customA precipitate formed
  4. customwas isolated by filtration
  5. washwashed with water
  6. customdried on the vacuum
  7. filtrationfilter funnel