HRID126994

反应详情

EQUATION

反应方程式

HRID 126994 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a stirred mixture of 9.8 g of (±)-4,5-dihydro-3-(2-thienyl)-1H-pyrazole-5-carboxylic acid (see example 2B) and 13.8 g of potassium carbonate in 80 ml of water and 40 ml of acetone there is added slowly 9.3 g of benzyl chloroformate dissolved in 50 ml of acetone, maintaining the temperature of the mixture at 10°-15° C. with an ice bath. After stirring at room temperature for 2 hours, the mixture is diluted with an equal volume of water and washed twice with ether. The aqueous layer containing some solids, is adjusted to pH 3.0 with 6 N HCl and cooled and filtered to obtain the title compound.

WORKUP

后处理

  1. temperaturemaintaining the temperature of the mixture at 10°-15° C. with an ice bath
  2. washwashed twice with ether
  3. additionThe aqueous layer containing some solids
  4. temperaturecooled
  5. filtrationfiltered