HRID220416

反应详情

EQUATION

反应方程式

HRID 220416 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
110 °C

PROCEDURE

实验过程

Charge a 2 L 3-neck round bottom flask with 2,3-dichloropyrazine (78.7 g, 0.532 mol), piperazine-1-carboxylic acid t-butyl ester (100 g, 0.537 mol), potassium carbonate (88.2 g, 0.638 mol) followed by DMA (0.780 L), and heat the resultant slurry to 110° C. under nitrogen with vigorous stirring. Cool to room temperature, add water (0.390 L) and MTBE (0.390 L), and stir the mixture for 60 min. Stop stirring and separate the layers. Wash the organic layer with water (2×200 mL), dry over MgSO4, filter and concentrate to give the title preparation as a yellow syrup (145 g, 91% yield).

WORKUP

后处理

  1. temperatureCool to room temperature
  2. stirringStop stirring
  3. customseparate the layers
  4. washWash the organic layer with water (2×200 mL)
  5. dry with materialdry over MgSO4
  6. filtrationfilter
  7. concentrationconcentrate
  8. customto give the title