Triethylene Glycol → 2-(4-Chlorobenzyl)-1-[4-(4-fluorophenyl)butyl]perhydroazepine

HRID 27435

Reaktionsgleichung

Reaktionsgleichung von HRID 27435
[Cl:1][C:2]1[CH:27]=[CH:26][C:5]([CH2:6][CH:7]2[CH2:13][CH2:12][CH2:11][CH2:10][CH2:9][N:8]2[CH2:14][CH2:15][CH2:16][C:17](=O)[C:18]2[CH:23]=[CH:22][C:21]([F:24])=[CH:20][CH:19]=2)=[CH:4][CH:3]=1.O.NN.[OH-].[K+].C(O)COCCOCCO>C(OCC)C.O>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([CH2:6][CH:7]2[CH2:13][CH2:12][CH2:11][CH2:10][CH2:9][N:8]2[CH2:14][CH2:15][CH2:16][CH2:17][C:18]2[CH:19]=[CH:20][C:21]([F:24])=[CH:22][CH:23]=2)=[CH:26][CH:27]=1

Komponenten

7

Edukt 4

HCID 8172Triethylene GlycolHCID 14797Potassium HydroxideHCID 24654Hydrazine hydrate (1:1)HCID 233428532-(4-Chlorobenzyl)-1-[3-(4-fluorobenzoyl)propyl]perhydroazepine

Produkt 1

HCID 233428342-(4-Chlorobenzyl)-1-[4-(4-fluorophenyl)butyl]perhydroazepineAusbeute 62,2 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 3283Diethyl EtherLösungsmittel

Versuchsvorschrift

Heat 0.5 g of the title compound of Example 39 with 1 ml of hydrazine hydrate, 0.5 g of potassium hydroxide and 5 ml of triglycol for 2 hours at 165°. Cool the resulting reaction mixture to ambient temperature. Mix the cooled reaction mixture with water and diethyl ether. Dry the ether phase over sodium sulfate and then concentrate it to obtain 0.3 g of the title compound as a viscous oil.

Aufarbeitung

  1. temperatureCool
  2. customthe resulting reaction mixture to ambient temperature
  3. additionMix
  4. dry with materialDry the ether phase over sodium sulfate
  5. concentrationconcentrate it

Quellen und Nachweise

ORD-Eintrag
ord-263ae71c66374e658004a1b702d7a9d6
Quelldatensatz
uspto-grants-1980_09
Patentnummer
US04221788

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