Water → HCID 58834682, compound

Participants

Reaction Steps

34.3 g (237 mmol) of 1-(2-hydroxyethyl)tetrahydropyrimidin-2(1H)-one (patent; Chem. Werke Huels; DE 1121617; 1962; Chem. Abstr.; EN; 56; 11601 g; 1962) are dissolved in 612 ml of DMF and admixed with 36.1 g (356 mmol) of triethylamine, 1.45 g (11.9 mmol) of DMAP and 85.0 g (309 mmol) of tert-butyl(chloro)diphenylsilane, and stirred at RT for 18 h. Then the mixture is added to 2000 ml of water and extracted three times with dichloromethane. The combined organic phases are washed twice with water and then dried over sodium sulfate. After filtration, the solvents are removed under reduced pressure. The residue is recrystallized from acetonitrile. This affords 71.9 g (78% of theory) of the desired compound.

Provenance & Evidence