反应 #94089

反应方程式

tetrahydrofuran

tetrahydrofuran

n-butyllithium

n-butyl bromide

1,3-dithiane

→

title compound

2-n-Butyl-1,3-dithiane

溶剂

n-hexane

反应条件

后处理

1. 1
   其他at -20° to -25° C
2. 2
   workup.STIRRINGwas stirred for 1 hour at -20° to -25° C. and for a further 30 minutes at room temperture
3. 3
   浓缩concentrated under reduced pressure
4. 4
   workup.DISSOLUTIONThe residue was dissolved in diethyl ether
5. 5
   洗涤washed with water
6. 6
   干燥an aqueous solution of sodium chloride, dried over magnesium sulphate
7. 7
   浓缩concentrated under reduced pressure
8. 8
   其他to give 6.8 g

实验过程

30 ml. of a 1.6M solution of n-butyllithium in n-hexane were added dropwise to a solution of 4.8 g. of 1,3-dithiane in 150 ml. of tetrahydrofuran under an atmosphere of nitrogen at -20° to -25° C. After 2 hours stirring, 6 g. of n-butyl bromide in 60 ml. of tetrahydrofuran were added dropwise to the reaction mixture, which was stirred for 1 hour at -20° to -25° C. and for a further 30 minutes at room temperture and then concentrated under reduced pressure. The residue was dissolved in diethyl ether, washed with water and an aqueous solution of sodium chloride, dried over magnesium sulphate and concentrated under reduced pressure to give 6.8 g. of the title compound having the following physical characteristics:

来源