Pyridine → HCID 58455273, 화합물

HRID 41821

반응식

HRID 41821 반응식
[Cl:1][C:2](Cl)([O:4]C(=O)OC(Cl)(Cl)Cl)Cl.[CH2:13]1[O:18][CH:17]([C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)[O:16][CH2:15][CH:14]1[OH:25].N1C=CC=CC=1>C(Cl)Cl>[C:2]([Cl:1])(=[O:4])[O:25][CH:14]1[CH2:13][O:18][CH:17]([C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)[O:16][CH2:15]1

참가 물질

5

반응물 3

HCID 1049PyridineHCID 743621,3-Dioxan-5-ol, 2-phenyl-HCID 94429Triphosgene2회

생성물 1

HCID 58455273HCID 58455273, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

반응 조건

온도
-40 °C

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

후처리

  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

출처 및 근거

ORD 기록
ord-88743db5226e4fbcacc170e4ad06550f
출처 데이터셋
uspto-grants-2013_09
특허 번호
US08535655B2

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