HRID37135

反应详情

EQUATION

反应方程式

HRID 37135 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

To a tetrahydrofuran suspension of 480 mg of 60% sodium hydride, 2 ml of ethyl formate and 1.0 g of ethyl methoxyacetate were added under nitrogen atmosphere, and the mixture was stirred for 16 hours at room temperature. In succession, adding 1.0 g of 3-amino-4(4-phenylthiophenyl)pyrazole, the solution was stirred for 4 hours in reflux. After allowing to cool, water was added and the solution was neutralized with 10% hydrochloric acid. Removing water, ethyl acetate was added, and insoluble matter was filtered. The filtrate was washed in ethyl acetate and ether and dried, and the title compound was obtained (100 mg, 8%).

WORKUP

后处理

  1. additionwere added under nitrogen atmosphere
  2. stirringthe solution was stirred for 4 hours
  3. temperaturein reflux
  4. temperatureto cool
  5. filtrationinsoluble matter was filtered
  6. washThe filtrate was washed in ethyl acetate
  7. dry with materialether and dried