Methyl vinyl ketone → HCID 86734689, Verbindung

HRID 329021

Reaktionsgleichung

Reaktionsgleichung von HRID 329021
[CH:1]([C:3]([CH3:5])=[O:4])=[CH2:2].[CH2:6]1[C@@H:16]2[C@H:10]([CH:11]=[CH:12][C:13]3[C:14]4[N:15]2[C:17]2[CH:26]=[CH:25][N:24]=[CH:23][C:18]=2[C:19]=4[CH2:20][CH2:21][CH:22]=3)[CH2:9][CH2:8][CH2:7]1>C(O)C>[CH2:6]1[CH:16]2[CH:10]([CH:11]=[CH:12][C:13]3[C:14]4[N:15]2[C:17]2[CH:26]=[CH:25][N:24]=[CH:23][C:18]=2[C:19]=4[CH2:20][CH2:21][CH:22]=3)[CH2:9][CH:8]([CH2:2][CH2:1][C:3](=[O:4])[CH3:5])[CH2:7]1

Komponenten

4

Edukt 2

HCID 6570Methyl vinyl ketone2×HCID 86734686(+/-)-trans-1,2,3,4,4a,8,9,14a-Octahydropyrido[4',3':2,3]indolo[1,7-ab][1]benzazepine

Produkt 1

HCID 86734689HCID 86734689, VerbindungAusbeute 86,5 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

2.3 grams of methyl vinyl ketone was added to a solution of 8.3 grams of (±)-trans-1,2,3,4,4a,8,9,14a-octahydropyrido[4',3':2,3]indolo[1,7-ab][1]benzazepine in 400 ml. of ethanol. The mixture was permitted to stand at room temperature for four days, after which an additional 2.6 grams of methyl vinyl ketone was added. This mixture was permitted to stand at room temperature for three days, and was then filtered, evaporated to dryness in vacuo, and triturated with pentane. The resulting solid was recrystallized from ethanol to yield 9 grams of the title compound with m.p. 102.5° C.

Aufarbeitung

  1. waitto stand at room temperature for three days
  2. filtrationwas then filtered
  3. customevaporated to dryness in vacuo
  4. customtriturated with pentane
  5. customThe resulting solid was recrystallized from ethanol

Quellen und Nachweise

ORD-Eintrag
ord-26158a1e72fa4421acd3e10164e0b61a
Quelldatensatz
uspto-grants-1977_04
Patentnummer
US04018930

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