HRID325080

反应详情

EQUATION

反应方程式

HRID 325080 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

5.8 g (23.4 mmol) of 2-ethoxymethyleneamino-3-carboethoxy-6-acetyl-4,5,6,7-tetrahydrothieno[2,3-c]pyridine in 50 ml of ethanol were mixed with 5.5 g (23.4 mmol) of 1-(2-aminoethyl)-4-(2-methoxyphenyl)piperazine and refluxed for 2 h. The mixture was then concentrated in a rotary evaporator, and the residue was taken up in 30 ml of ethyl acetate, heated to boiling and left to cool with stirring. The solid which crystallized out was filtered off with suction after cooling in an ice bath and was washed with ethyl acetate. 8.7 g (80%) of product with melting point 170-172° C. were isolated.

WORKUP

后处理

  1. temperaturerefluxed for 2 h
  2. concentrationThe mixture was then concentrated in a rotary evaporator
  3. temperatureheated
  4. waitleft
  5. temperatureto cool
  6. customThe solid which crystallized out
  7. filtrationwas filtered off with suction
  8. temperatureafter cooling in an ice bath
  9. washwas washed with ethyl acetate