Chlorotrimethylsilane → Diethyl trimethylsilyl phosphite

To a mixture of diethyl phosphite (2.8 mL, 0.0217 mol) and triethylamine (9.mL, 0.065 mol, 3.0 equiv.) in dry diethyl ether (250 mL) at 0° C. was slowly added freshly distilled trimethylsilyl chloride (3.3 mL, 0.0260 mol, 1.2 equiv.) via syringe. The resulting slurry was allowed to slowly warm to room temperature, and was then warmed to 45° C. for 14 h. Volatiles were removed by distillation using a 55° C. oil bath. The resulting mixture was diluted with pentane (150 mL), filtered to remove triethylammonium salts, and concentrated at atmospheric pressure using a 55° C. oil bath. Distillation of the resulting oil gave diethyl trimethylsilyl phosphite as a colorless oil (3.64 g, 80%).

1. temperaturewas then warmed to 45° C. for 14 h
2. customVolatiles were removed by distillation
3. customusing a 55° C.
4. additionThe resulting mixture was diluted with pentane (150 mL)
5. filtrationfiltered
6. customto remove triethylammonium salts
7. concentrationconcentrated at atmospheric pressure
8. customusing a 55° C.
9. distillationDistillation of the resulting oil

ORD record

ord-bf8bb56d57114178b5fd76cdd04d3527

Source dataset

uspto-grants-1999_02

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05874473