HRID1400301

反应详情

EQUATION

反应方程式

HRID 1400301 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 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

  1. temperatureThe resulting mixture was heated
  2. temperatureat reflux overnight
  3. customAfter TLC control (n-hexane/ethyl acetate 65:35), solvent was evaporated in vacuo
  4. dissolutionthe residue was dissolved in 15 mL of ethyl acetate
  5. washwashed with water (3×5 mL), brine (10 mL)
  6. dry with materialdried over Na2SO4
  7. customThe evaporation of solvent