تفاعل #78328

معادلة التفاعل

trimethylsilyl bromide

compound 2

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

→

bight yellow oil

المردود 100.0%

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

المردود 100.0%

ظروف التفاعل

المعالجة

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

الإجراء التجريبي

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%.

المصدر