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
In 10 mL of N,N-dimethylformamide was dissolved 1.0 g of 3,6-difluoro-2-pyrazinecarbonitrile. At an ice-cooled temperature, 0.64 g of sodium acetate was added and stirred for 6 hours. The reaction mixture was added to a mixture of 20 mL of ethyl acetate and 20 mL of water, pH was adjusted to 1.5 with 6 mol/L hydrochloric acid, and the organic layer was separated. The organic layer was washed with saturated aqueous solution of sodium chloride and dried on anhydrous magnesium sulfate, and the solvent was removed under reduced pressure. The residue thus obtained was purified by silica gel chromatography [eluent: n-hexane:ethyl acetate-: 1:1] to obtain 0.45 g of 6-fluoro-3-oxo-3,4-dihydro-2-pyrazinecarbonitrile as a yellow-colored solid product.
WORKUP
后处理
- additionwas added
- customthe organic layer was separated
- washThe organic layer was washed with saturated aqueous solution of sodium chloride
- dry with materialdried on anhydrous magnesium sulfate
- customthe solvent was removed under reduced pressure
- customThe residue thus obtained
- customwas purified by silica gel chromatography [eluent: n-hexane:ethyl acetate-: 1:1]