反应 #1519101

反应方程式

Tetrabromomethane

7-oxanorborn-2-en-5-ylmethanol

triphenylphosphine

→

7-oxanorborn-2-en-5-yl-methyl bromide

溶剂

CH2Cl2

反应条件

后处理

1. 1
   温度to warm to room temperature
2. 2
   其他The solvent was removed under reduced pressure
3. 3
   其他The crude product was purified by flash chromatography (
4. 4
   workup.ADDITIONa 98:2 mixture of cyclohexane and ethyl acetate)
5. 5
   其他0.3 g (59% of theory) of the pure product were obtained

实验过程

Tetrabromomethane (1.161 g, 3.50 mmol) was added to a solution of 7-oxanorborn-2-en-5-ylmethanol (0.305 g, 2.50 mmol, from Example 2) in CH2Cl2 (12.5 ml). The solution was cooled to 0° C. and admixed with triphenylphosphine (1.836 g, 7 mmol). The reaction mixture was allowed to warm to room temperature and stirred for 12 h. The solvent was removed under reduced pressure and the remaining solid was taken up in cyclohexane. The crude product was purified by flash chromatography (using a 98:2 mixture of cyclohexane and ethyl acetate). 0.3 g (59% of theory) of the pure product were obtained. The product was stored under cool conditions with the exclusion of light.

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