HRID1400301
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 5-chloro-6-hydroxynaphthalene-2-carbonitrile (1.5 mmol) and K2CO3 (3 mmol) in acetone was added tert-butyl (2-bromoethyl)carbamate (2.1 mmol). The resulting mixture was heated at reflux overnight. After TLC control (n-hexane/ethyl acetate 65:35), solvent was evaporated in vacuo and the residue was dissolved in 15 mL of ethyl acetate and washed with water (3×5 mL), brine (10 mL) and dried over Na2SO4. The evaporation of solvent afforded tert-butyl {2-[(1-chloro-6-cyanonaphthalen-2-yl)oxy]ethyl}carbamate as a brown solid (81% yield) which was used without further purification.
WORKUP
后处理
- temperatureThe resulting mixture was heated
- temperatureat reflux overnight
- customAfter TLC control (n-hexane/ethyl acetate 65:35), solvent was evaporated in vacuo
- dissolutionthe residue was dissolved in 15 mL of ethyl acetate
- washwashed with water (3×5 mL), brine (10 mL)
- dry with materialdried over Na2SO4
- customThe evaporation of solvent