반응 #70099

반응 방정식

pyridine

Triphosgene

bis(trichloromethyl)carbonate

1,3-O-benzylideneglycerol

→

2-phenyl-1,3-dioxan-5-yl carbonochloridate

용매

CH2Cl2

반응 조건

후처리

1. 1
   workup.ADDITIONUpon completion of the addition the reaction mixture
2. 2
   workup.STIRRINGwas stirred for 30 min at −40° C
3. 3
   온도to warm to 0° C. over 60 min
4. 4
   온도subsequently warmed to rt over 3.5 h
5. 5
   workup.STIRRINGunder stirring
6. 6
   기타The reaction product was used in the next step without any further purification

실험 절차

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

출처