HRID617178

反应详情

EQUATION

反应方程式

HRID 617178 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To an ice-cold solution of 2-amino-4-(4-piperidyl)quinazoline (500 mg, 2.19 mmol) and triethylamine (233 mg, 2.3 mmol) in N,N-dimethylformamide (10 ml) was added dropwise acetic anhydride (0.22 ml, 2.30 mmol) under a nitrogen atmosphere. The reaction mixture was stirred for about 3 hours and was evaporated. The residue was partitioned between dichloromethane and saturated sodium hydrogencarbonate aqueous solution. The organic layer was washed with water and then dried over sodium sulfate and evaporated in vacuo. The residue was crystallized from ethanol. Recrystallization from methanol gave the titled compound(452 mg).

WORKUP

后处理

  1. customwas evaporated
  2. customThe residue was partitioned between dichloromethane and saturated sodium hydrogencarbonate aqueous solution
  3. washThe organic layer was washed with water
  4. dry with materialdried over sodium sulfate
  5. customevaporated in vacuo
  6. customThe residue was crystallized from ethanol
  7. customRecrystallization from methanol