HRID231772

反应详情

EQUATION

反应方程式

HRID 231772 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Grams 7.4 of 1-(2,3-dihydroxypropyl)piperazine and 4.3 g of 4-chloropyrimidine-5-carboxylic acid ethyl ester were warmed to 90° C. for 45 minutes in 100 ml dioxane. The reaction mixture was then settled, the supernatant liquor evaporated to dryness and the residue dissolved in hydrochloric ethanol and diluted with isopropanol until complete precipitation. By addition of 95° ethanol, the so formed gum crystallized and 4 g of 4-[4-(2,3-dihydroxypropyl)piperazin-1-yl]pyrimidine-5-carboxylic acid ethyl ester dihydrochloride, melting at 190°-193° C. (with decomposition), were obtained.

WORKUP

后处理

  1. customthe supernatant liquor evaporated to dryness
  2. dissolutionthe residue dissolved in hydrochloric ethanol
  3. additiondiluted with isopropanol until complete precipitation
  4. additionBy addition of 95° ethanol
  5. customthe so formed gum crystallized