HRID1427152

反应详情

EQUATION

反应方程式

HRID 1427152 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of bis(1,1-dimethylethyl) 2-[3-(ethyloxy)-3-oxopropanoyl]-1,4-piperazinedicarboxylate (may be prepared as described in Intermediate 3; 7.2 g) in ethanol (250 mL) was added ammonium acetate (6.93 g). The reaction mixture was heated to reflux for 7 hours and then left to stand at room temperature overnight. The reaction mixture was evaporated and then partitioned between 2× EtOAc and water. The combined organic phases were washed with water, dried through a hydrophobic frit and evaporated to give the title compound as a yellow oil (7.40 g).

WORKUP

后处理

  1. temperatureThe reaction mixture was heated
  2. temperatureto reflux for 7 hours
  3. waitleft
  4. customThe reaction mixture was evaporated
  5. custompartitioned between 2× EtOAc and water
  6. washThe combined organic phases were washed with water
  7. customdried through a hydrophobic frit
  8. customevaporated