تفاعل #575348

معادلة التفاعل

diethyl hydroxylmethylphosphonate

triethylamine

dimethylaminopyridine

t-butyldimethylsilyl chloride

→

title compound

Diethyl (t-Butyldimethylsiloxy)methylphosphonate

المذيبات

dichlormethane

dichloromethane

water

ظروف التفاعل

المعالجة

1. 1
   استخلاصextracted with dichloromethane (2×100 ml)
2. 2
   تجفيفThe organic extracts were dried (Na2SO4)
3. 3
   تركيزconcentrated in vacuo
4. 4
   أخرىthe resulting oil chromatographed on silica gel
5. 5
   غسيلeluted with ethylacetate:hexanes (1:1, v:v)

الإجراء التجريبي

To a stirred solution of diethyl hydroxylmethylphosphonate (2.13 g, 12.7 mmol), triethylamine (2.12 ml, 15.2 mmol) and dimethylaminopyridine (77 mg, 0.63 mmol) in dichlormethane at 0° C. under argon, at r.t., was added t-butyldimethylsilyl chloride (1.85 g, 12.8 mmol) in dichloromethane (5 ml). After 14 hr the resulting slurry was poured into water (100 ml) and extracted with dichloromethane (2×100 ml). The organic extracts were dried (Na2SO4), concentrated in vacuo and the resulting oil chromatographed on silica gel eluted with ethylacetate:hexanes (1:1, v:v) to afford the title compound as a clear oil.

المصدر