1,4-Dichlorobutane → 8-Aza-5-azoniaspiro(4.5)decane, 8-(2-pyrimidinyl)-, bromide (1:1)

HRID 1703341

Reaktionsgleichung

Reaktionsgleichung von HRID 1703341
[N:1]1[CH:6]=[CH:5][CH:4]=[N:3][C:2]=1[N:7]1[CH2:12][CH2:11][NH:10][CH2:9][CH2:8]1.Cl[CH2:14][CH2:15][CH2:16][CH2:17]Cl.O.C(=O)([O-])[O-].[Na+].[Na+].[Br-:26].[K+]>C(O)(C)C>[Br-:26].[N:1]1[CH:6]=[CH:5][CH:4]=[N:3][C:2]=1[N:7]1[CH2:12][CH2:11][N+:10]2([CH2:17][CH2:16][CH2:15][CH2:14]2)[CH2:9][CH2:8]1

Komponenten

6

Edukt 4

HCID 80591,4-DichlorobutaneHCID 887471-(2-Pyrimidinyl)piperazineHCID 253877Potassium BromideHCID 2735133Sodium Carbonate Monohydrate

Produkt 1

HCID 6575058-Aza-5-azoniaspiro(4.5)decane, 8-(2-pyrimidinyl)-, bromide (1:1)

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 3776IsopropanolLösungsmittel

Versuchsvorschrift

A mixture of 1-(2-pyrimidinyl)piperazine (16.4 g., 0.1 mole), 1,4-dichlorobutane (23.8 g., 0.19 mole), sodium carbonate monohydrate (30.8 g., 0.25 mole) and potassium bromide (44.6 g., 0.375 mole) in 150 ml. of isopropanol is stirred and refluxed for an 8-hr. period. The hot reaction mixture is filtered and insolubles washed with hot isopropanol. Concentration of the combined filtrates under reduced pressure and trituration of residual material with acetone provides 8-(2-pyrimidinyl)-8-aza-5-azoniaspiro[4.5]decane bromide in yields of 50-90%.

Aufarbeitung

  1. temperaturerefluxed for an 8-hr
  2. filtrationThe hot reaction mixture is filtered
  3. washinsolubles washed with hot isopropanol

Quellen und Nachweise

ORD-Eintrag
ord-c2029de5b9f94c18bcc626a10bdb61ff
Quelldatensatz
uspto-grants-1982_09
Patentnummer
US04351939

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