Ethanol → HCID 3035775, compound

Participants

Reaction Steps

23 ml of trimethylbromosilane are added dropwise at room temperature withina period of 15 minutes to a solution of 10.3 g of 4 according to b) in 42 ml of dichloromethane. After 211/2 hours, 42 ml of ethanol are added whilecooling with ice, and the mixture is stirred for 20 hours. The whole is then concentrated by evaporation and the residue is dissolved three times in 70 ml of toluene each time and in each case is concentrated by evaporation again. The residue is dissolved in 42 ml of ethanol, and 42 mlof propylene oxide are added. After 11/2 hours, the mixture is filtered. Drying the filtration residue in a vacuum desiccator over P2O5 /KOH (3 hours/80°) yields 6.17 g of 5; [α]D =-78°(c=0.6, H2O); m.p. 194°-197° (decomp.), C8H16NO5P; calculated: C 40.51%, H 6.80%, N 5.91%, P 13.06%; found: C 39.4%, H 7.09%, N 5.73%, P 12.98%.

Provenance & Evidence