反应 #78328

反应方程式

trimethylsilyl bromide

compound 2

2-[4-(dimethoxyphosphoryl)-2-oxabutyl]-acrylic acid diethylamide

→

bight yellow oil

收率 100.0%

2-[4-(dihydroxyphosphoryl)-2-oxabutyl]-acrylic acid diethylamide

收率 100.0%

反应条件

后处理

1. 1
   浓缩Afterwards, it is firstly concentrated in a water-jet vacuum
2. 2
   workup.ADDITIONin a fine vacuum (0.2 mbar), 70 ml of absolute methanol are added
3. 3
   workup.STIRRINGthe mixture is stirred overnight at room temperature
4. 4
   浓缩The slightly yellowish, clear solution is concentrated on the rotary evaporator
5. 5
   其他dried off in fine vacuum (0.2 mbar) at 40° C. until its weight

实验过程

17 g (111 mmol) trimethylsilyl bromide are slowly added dropwise to 13.5 g (51 mmol) of compound 2 and the mixture is subsequently stirred for 2 hours at 40° C. Afterwards, it is firstly concentrated in a water-jet vacuum and then in a fine vacuum (0.2 mbar), 70 ml of absolute methanol are added and the mixture is stirred overnight at room temperature. The slightly yellowish, clear solution is concentrated on the rotary evaporator and dried off in fine vacuum (0.2 mbar) at 40° C. until its weight is constant. 13.5 g (100% yield) of a bight yellow oil remain as product, which has a HPLC purity of 98.1%.

来源