HRID622309
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
PROCEDURE
实验过程
A mixture of 37 parts of methyl N-[phenyl(2-pyridinyl)methyl]glycine, 36 parts of formic acid and 450 parts of dimethylbenzene was stirred and refluxed for 2 hours. The reaction mixture was poured into water. The product was extracted with 1,1'-oxybisethane. The extract was washed successively with a sodium hydroxide solution 10% and water, dried, filtered and evaporated. The residue was purified by column chromatography over silica gel using a mixture of trichloromethane and methanol (90:10 by volume) as eluent. The pure fractions were collected and the eluent was evaporated, yielding 24 parts (60.3%) of methyl N-formyl-N-[phenyl(2-pyridinyl)methyl]glycine as a residue.
WORKUP
后处理
- temperaturerefluxed for 2 hours
- extractionThe product was extracted with 1,1'-oxybisethane
- washThe extract was washed successively with a sodium hydroxide solution 10% and water
- customdried
- filtrationfiltered
- customevaporated
- customThe residue was purified by column chromatography over silica gel using
- additiona mixture of trichloromethane and methanol (90:10 by volume) as eluent
- customThe pure fractions were collected
- customthe eluent was evaporated