Ethanol → HCID 12874074, Verbindung

HRID 461558Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 461558
Cl.[CH3:2][N:3]([CH3:11])[CH:4]1[CH2:9][CH2:8][C:7](=O)[CH2:6][CH2:5]1.Cl.[CH2:13]([O:20][C:21]1[CH:22]=[C:23]([NH:27]N)[CH:24]=[CH:25][CH:26]=1)[C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1.C(O)C>O>[CH3:2][N:3]([CH3:11])[CH:4]1[CH2:9][C:8]2[C:24]3[C:23](=[CH:22][C:21]([O:20][CH2:13][C:14]4[CH:15]=[CH:16][CH:17]=[CH:18][CH:19]=4)=[CH:26][CH:25]=3)[NH:27][C:7]=2[CH2:6][CH2:5]1

Komponenten

5

Edukt 3

HCID 702EthanolHCID 127174484-(Dimethylamino)cyclohexan-1-one--hydrogen chloride (1/1)HCID 12891839(3-(Benzyloxy)phenyl)hydrazine hydrochloride

Produkt 1

HCID 12874074HCID 12874074, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

A solution of 15.8 g. of 4-dimethylaminocyclohexanone hydrochloride and 20.3 g. of 3-benzyloxyphenylhydrazine hydrochloride (m.p. 165°-168° C.) in 225 ml. of absolute ethyl alcohol was heated under reflux for three hours, cooled to room temperature, and diluted with 50 ml. of water. After standing for three hours the resulting crystals were collected by filtration and washed with ethyl alcohol to give, after recrystallization from ethyl alcohol, 6.1 g. of 3-(dimethylamino)-7-(benzyloxy)-1,2,3,4-tetrahydrocarbazole hydrochloride, m.p. 237°-239° C.

Aufarbeitung

  1. temperatureunder reflux for three hours
  2. additiondiluted with 50 ml
  3. filtrationthe resulting crystals were collected by filtration
  4. washwashed with ethyl alcohol
  5. customto give
  6. customafter recrystallization from ethyl alcohol, 6.1 g

Quellen und Nachweise

ORD-Eintrag
ord-dc411932b4a94c0084520834d420f485
Quelldatensatz
uspto-grants-1977_12
Patentnummer
US04062864

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