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 suspension of 8-(2,6-dimethyl-3-nitrobenzyloxy)-2-methylquinoline (2.34 g), ferric chloride (70.6 mg) and carbon (70.6 mg) in methanol (35 ml) was added hydrazine monohydrate (1.09 g) at 65° C., and the mixture was refluxed for 2 hours. Methanol (20 ml) was added thereto, and the mixture was refluxed for 1 hour. After cooling chloroform was added thereto, and the resulting precipitates were filtered off. The filtrate was concentrated and the residue was dissolved in chloroform. The solution was washed with saturated sodium bicarbonate solution, water and brine, dried over magnesium sulfate and concentrated. The residue was crystallized with ethyl acetate to give 8-(3-Amino-2,6-dimethylbenzyloxy)-2-methylquinoline (1.67 g) as a pale crystal.
WORKUP
后处理
- temperaturethe mixture was refluxed for 2 hours
- temperaturethe mixture was refluxed for 1 hour
- additionwas added
- customthe resulting precipitates
- filtrationwere filtered off
- concentrationThe filtrate was concentrated
- dissolutionthe residue was dissolved in chloroform
- washThe solution was washed with saturated sodium bicarbonate solution, water and brine
- dry with materialdried over magnesium sulfate
- concentrationconcentrated
- customThe residue was crystallized with ethyl acetate