HRID444163

反应详情

EQUATION

反应方程式

HRID 444163 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Dissolve the acid chloride from Step A in 20 ml. of dry tetrahydrofuran and add this solution dropwise with stirring to a cooled (ice-bath) saturated solution of ammonia in 60 ml of tetrahydrofuran. Pass ammonia through the reaction mixture simultaneously for 15 minutes. Stir at room temperature for an additional 15 minutes and evaporate the reaction mixture to dryness. Add a mixture of 12 ml of ethanol and 60 ml of water to the residue and stir at room temperature for an additional 30 minutes. Separate the solid by filtration and wash with water, then with ethanol and then with ether. Dry in vacuo to obtain the title product.

WORKUP

后处理

  1. stirringStir at room temperature for an additional 15 minutes
  2. customevaporate the reaction mixture to dryness
  3. additionAdd
  4. additiona mixture of 12 ml of ethanol and 60 ml of water to the residue
  5. stirringstir at room temperature for an additional 30 minutes
  6. customSeparate the solid
  7. filtrationby filtration
  8. washwash with water
  9. customDry in vacuo