Water → HCID 86734685, Verbindung

HRID 329018

Reaktionsgleichung

Reaktionsgleichung von HRID 329018
[CH2:1]1[C@@H:11]2[C@H:5]([CH:6]=[CH:7][C:8]3[C:9]4[N:10]2[C:12]2[CH:21]=[CH:20][N:19]=[CH:18][C:13]=2[C:14]=4[CH2:15][CH2:16][CH:17]=3)[CH2:4][CH2:3][CH2:2]1.C(N(CC)CC)C.Cl[CH2:30][CH:31]=[C:32]([Cl:34])[CH3:33].O>CN(C)C=O>[Cl:34][C:32]([CH3:33])=[CH:31][CH2:30][CH:3]1[CH2:4][CH:5]2[CH:6]=[CH:7][C:8]3[C:9]4[N:10]([C:12]5[CH:21]=[CH:20][N:19]=[CH:18][C:13]=5[C:14]=4[CH2:15][CH2:16][CH:17]=3)[CH:11]2[CH2:1][CH2:2]1

Komponenten

6

Edukt 4

HCID 962WaterHCID 8471TriethylamineHCID 135561,3-Dichloro-2-buteneHCID 86734686(+/-)-trans-1,2,3,4,4a,8,9,14a-Octahydropyrido[4',3':2,3]indolo[1,7-ab][1]benzazepine

Produkt 1

HCID 86734685HCID 86734685, VerbindungAusbeute 80,4 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

A suspension of 2.76 g of (±)-trans-1,2,3,4,4a,8,9,14a-octahydropyrido[4',3';2,3]indolo[1,7-ab][1]benzazepine in 20 ml of dimethylformamide (DMF) containing 2.3 ml triethylamine was treated with 1.25 g of 1,3-dichloro-2-butene. Solution resulted immediately. The solution was stirred at room temperature for 4 hours, by which time some white precipitate had formed. The reaction mixture was poured into 150 ml of cold water, a gummy solid was separated and washed by decantation with cold water. Recrystallization from ethanol gave 2.93 g of the title compound, m.p. 130°-132° C.

Aufarbeitung

  1. customSolution resulted immediately
  2. customhad formed
  3. customa gummy solid was separated
  4. washwashed by decantation with cold water
  5. customRecrystallization from ethanol

Quellen und Nachweise

ORD-Eintrag
ord-056e9fa4c4734dc388454b9a3f610f02
Quelldatensatz
uspto-grants-1977_04
Patentnummer
US04018930

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