HRID494336

反应详情

EQUATION

反应方程式

HRID 494336 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of methyl 2-[(2′-cyanobiphenyl-4-yl)methylamino]-3-methoxycarbonylaminobenzoate (10.5 g) in methanol (100 ml) was added NaOMe (10 g), and the mixture was heated under reflux for 20 hours. The reaction mixture was neutralized with 1N-HCl and concentrated to dryness. The residue was extracted with chloroform-water. The organic layer was washed with water, dried and evaporated to dryness. The resulting crystals were recrystallized from chloroform-methanol to afford colorless needles (8.67 g, 89%), m.p. 250-253° C.

WORKUP

后处理

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 20 hours
  3. concentrationconcentrated to dryness
  4. extractionThe residue was extracted with chloroform-water
  5. washThe organic layer was washed with water
  6. customdried
  7. customevaporated to dryness
  8. customThe resulting crystals were recrystallized from chloroform-methanol