HRID1040372

反应详情

EQUATION

反应方程式

HRID 1040372 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
20 °C

PROCEDURE

实验过程

Add 1.79 g (10.05 mmol) of N-bromosuccinimide to a solution of 1.4 g (9.14 mmol) of methyl 5-aminopyrazine-2-carboxylate in 10 mL of acetonitrile. Stir the reaction mixture for 2 h at 20° C. then distribute in 100 mL of EtOAc/water 1:1 mixture. Wash the organic phase with 2×50 mL of water, dry over Na2SO4 and concentrate under reduced pressure. Purify the residue obtained by silica gel column chromatography, eluting with a cyclohexane/EtOAc gradient from 0 to 50% of EtOAc. After concentration under reduced pressure, we obtain 1.66 g of methyl 5-amino-6-bromopyrazine-2-carboxylate in the form of yellow wax.

WORKUP

后处理

  1. washWash the organic phase with 2×50 mL of water
  2. dry with materialdry over Na2SO4
  3. concentrationconcentrate under reduced pressure
  4. customPurify the residue
  5. customobtained by silica gel column chromatography
  6. washeluting with a cyclohexane/EtOAc gradient from 0 to 50% of EtOAc
  7. concentrationAfter concentration under reduced pressure, we