HRID422219

反应详情

EQUATION

反应方程式

HRID 422219 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Combine 4-(5-Oxo-5,6,7,8-tetrahydro-naphthalen-2-yloxy)-benzonitrile (5.34, 20.3 mmol), t-butyl alcohol (100 ml), and KOH (5.7 g, 101.5 mmol). After the reaction stirs for 72 hours at room temperature, concentrate under reduced pressure and then add ethyl acetate. Wash the organic phase with water, a brine solution, and then dry the organic layer over Na2SO4. Flash chromatograph using 2/1 CH2Cl2/ethyl acetate eluent to afford 5.20 g, 18.5 mmol (91% yield) of the title compound: 1H NMR (500 MHz, CDCl3); 2.1-2.2 (2H, m), 2.6-2.7 (2H, m), 2.9-3.0 (2H, m), 5.6-6.2 (2H, br m); 6.85 (1H, s), 6.9-7.0 (1H, m), 7.05-7.15 (2H, m), 7.8-7.9 (2H, m) 8.05-8.10 (1H, m); MS m/z 284 (M+3).

WORKUP

后处理

  1. concentrationconcentrate under reduced pressure
  2. washWash the organic phase with water
  3. dry with materiala brine solution, and then dry the organic layer over Na2SO4