HRID1582695

反应详情

EQUATION

反应方程式

HRID 1582695 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 3-(4′-chloro-[1,1′-biphenyl]4yl)-2-butenol (4g, 500 gm) and methylene blue (40 mg) in CH3CN (30 ml) was photooxygenated at 5° C. for 5 h. Cyclopentanone (0.5 ml) and hydrochloric acid (5 drops) were added and reaction mixture was stirred at r.t. for 1.5 h and then left at r.t for 48 h. The reaction mixture was concentrated. Crude product was purified by column chromatography to furnish 230 mg (33.8% yield, based on allylic alcohol, 4g used) of trioxane 7ga m.p. 105-107° C.

WORKUP

后处理

  1. customreaction mixture
  2. waitleft at r.t for 48 h
  3. concentrationThe reaction mixture was concentrated
  4. customCrude product was purified by column chromatography
  5. customto furnish 230 mg (33.8% yield