Water → HCID 68687571, Verbindung

HRID 2244216Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2244216
[C:1]1([C:23]2[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=2)[CH:6]=[CH:5][C:4]([C:7]([N:9]2[C:15]3[CH:16]=[CH:17][CH:18]=[CH:19][C:14]=3[CH2:13][N:12]3[CH:20]=[CH:21][CH:22]=[C:11]3[CH2:10]2)=[O:8])=[CH:3][CH:2]=1.[Cl:29][C:30]([Cl:35])([Cl:34])[C:31](Cl)=[O:32].O>O1CCOCC1>[C:1]1([C:23]2[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=2)[CH:2]=[CH:3][C:4]([C:7]([N:9]2[C:15]3[CH:16]=[CH:17][CH:18]=[CH:19][C:14]=3[CH2:13][N:12]3[C:20]([C:31](=[O:32])[C:30]([Cl:35])([Cl:34])[Cl:29])=[CH:21][CH:22]=[C:11]3[CH2:10]2)=[O:8])=[CH:5][CH:6]=1

Komponenten

5

Edukt 3

HCID 962WaterHCID 6420Trichloroacetyl chlorideHCID 9799174HCID 9799174, Verbindung

Produkt 1

HCID 68687571HCID 68687571, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 312751,4-DioxaneLösungsmittel

Versuchsvorschrift

10-(1,1′-Biphenyl-4-ylcarbonyl)-10,11-dihydro-5H-pyrrolo[2,1-c][1,4]benzodiazepine of Step A (1.822 g; 0.005 mol) was dissolved in 50 mL of 1,4-dioxane to which was then added 0.946 g (0.0052 mol) of trichloroacetyl chloride. The reaction solution was heated under reflux with stirring over night, cooled to room temperature and then poured into 250 mL of water. Recrystallization of the crude material from ethanol provided a solid, m.p. 197-198° C.

Aufarbeitung

  1. temperatureThe reaction solution was heated
  2. temperatureunder reflux
  3. customRecrystallization of the crude material from ethanol
  4. customprovided a solid, m.p. 197-198° C.

Quellen und Nachweise

ORD-Eintrag
ord-e83aa627fea141a297d2ee9749e36791
Quelldatensatz
uspto-grants-2010_03
Patentnummer
US07678787B2

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