Pyridine → HCID 58455273, Verbindung

HRID 41821Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 41821
[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

Komponenten

5

Edukt 3

HCID 1049PyridineHCID 743621,3-Dioxan-5-ol, 2-phenyl-HCID 94429Triphosgene2×

Produkt 1

HCID 58455273HCID 58455273, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Reaktionsbedingungen

Temperatur
-40 °C

Versuchsvorschrift

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

Aufarbeitung

  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

Quellen und Nachweise

ORD-Eintrag
ord-88743db5226e4fbcacc170e4ad06550f
Quelldatensatz
uspto-grants-2013_09
Patentnummer
US08535655B2

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