反応 #78328

反応方程式

trimethylsilyl bromide

compound 2

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

→

bight yellow oil

収率 100.0%

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

収率 100.0%

反応条件

後処理

1. 1
   濃縮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
   濃縮The slightly yellowish, clear solution is concentrated on the rotary evaporator
5. 5
   その他dried off in fine vacuum (0.2 mbar) at 40° C. until its weight

実験手順

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%.

出典