反应详情

温度

-40 °C

Triphosgene (bis(trichloromethyl)carbonate (13.35 g, 45.0 mmol) was added under argon at room temperature to a solution of 1,3-O-benzylideneglycerol (18.02 g, 100.0 mmol) in dry CH2Cl2 (300 ml). The reaction mixture was cooled to −40° C. and a solution of pyridine (10.9 ml, 135.0 mmol) was added over 35 min under stirring. Upon completion of the addition the reaction mixture was stirred for 30 min at −40° C. Then it was allowed to warm to 0° C. over 60 min and subsequently warmed to rt over 3.5 h under stirring. The reaction product was used in the next step without any further purification

1. additionUpon completion of the addition the reaction mixture
2. stirringwas stirred for 30 min at −40° C
3. temperatureto warm to 0° C. over 60 min
4. temperaturesubsequently warmed to rt over 3.5 h
5. stirringunder stirring
6. customThe reaction product was used in the next step without any further purification