HRID1614009

反应详情

EQUATION

反应方程式

HRID 1614009 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Potassium hydroxide (400 mg, 7.0 mmole) was added to a solution of 1,2-diphenylethane-l,2-diol (I40 mg, 0.65 mmole) in dry ether (30 mL). TsCl (286 mg, 1.5 mmole) was added. The reaction was completed after 1 hour with stirring under N2 atmosphere at RT. A white solid was obtained. The white solid was filtered and washed with dichloromethane. The combined filtrate was concentrated, Recrystallization with methylene chloride and hexane gave the crystalline solid (1.4 g, 44.6%), mp, 110-112 (decomposed), 'H-NMR(CDCl3) δ, 2.39(s, 6H CH3), 5.61(s, 2H, CH), 6.89-7.55(m, 18H, ArH).

WORKUP

后处理

  1. customA white solid was obtained
  2. filtrationThe white solid was filtered
  3. washwashed with dichloromethane
  4. concentrationThe combined filtrate was concentrated
  5. customRecrystallization with methylene chloride and hexane