HRID622309

反应详情

EQUATION

反应方程式

HRID 622309 的结构方程式

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

  1. temperaturerefluxed for 2 hours
  2. extractionThe product was extracted with 1,1'-oxybisethane
  3. washThe extract was washed successively with a sodium hydroxide solution 10% and water
  4. customdried
  5. filtrationfiltered
  6. customevaporated
  7. customThe residue was purified by column chromatography over silica gel using
  8. additiona mixture of trichloromethane and methanol (90:10 by volume) as eluent
  9. customThe pure fractions were collected
  10. customthe eluent was evaporated