HRID1040371

反应详情

EQUATION

反应方程式

HRID 1040371 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Reflux a solution of 2.24 g (18.65 mmol) of 5-aminopyrazine-2-carbonitrile and 9.45 mL (74.40 mmol) of boron trifluoride etherate in 50 mL of methanol for 2 h. Concentrate the reaction mixture under reduced pressure and take up the residue obtained in 200 mL of EtOAc and 10 mL of a saturated aqueous solution of NaHCO3. Dry the organic phase over Na2SO4 and concentrate under reduced pressure. Purify the residue obtained by silica gel column chromatography, eluting with a cyclohexane/EtOAc 1:1 mixture. After concentration under reduced pressure, we obtain 1.4 g of methyl 5-aminopyrazine-2-carboxylate in the form of oil.

WORKUP

后处理

  1. concentrationConcentrate the reaction mixture under reduced pressure
  2. customobtained in 200 mL of EtOAc
  3. dry with materialDry the organic phase over Na2SO4
  4. concentrationconcentrate under reduced pressure
  5. customPurify the residue
  6. customobtained by silica gel column chromatography
  7. washeluting with a cyclohexane/EtOAc 1:1 mixture
  8. concentrationAfter concentration under reduced pressure, we