HRID1040371
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- concentrationConcentrate the reaction mixture under reduced pressure
- customobtained in 200 mL of EtOAc
- dry with materialDry the organic phase over Na2SO4
- concentrationconcentrate under reduced pressure
- customPurify the residue
- customobtained by silica gel column chromatography
- washeluting with a cyclohexane/EtOAc 1:1 mixture
- concentrationAfter concentration under reduced pressure, we