반응 #78328

반응 방정식

trimethylsilyl bromide

compound 2

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

→

bight yellow oil

수율 100.0%

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

수율 100.0%

반응 조건

후처리

1. 1
   농축Afterwards, 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
   농축The slightly yellowish, clear solution is concentrated on the rotary evaporator
5. 5
   기타dried off in fine vacuum (0.2 mbar) at 40° C. until its weight

실험 절차

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%.

출처