HRID860929
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
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
- temperaturethe mixture was heated
- temperatureunder reflux for 20 hours
- concentrationconcentrated to dryness
- extractionThe residue was extracted with chloroform-water
- washThe organic layer was washed with water
- customdried
- customevaporated to dryness
- customThe resulting crystals were recrystallized from chloroform-methanol