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

HRID 1649474

反応式

HRID 1649474 の反応式
[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

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒

実験手順

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%.

後処理

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

出典と根拠

ORDレコード
ord-a03b86e1e8234b339a0b5bb7f3a065b2
出典データセット
uspto-grants-1983_11
特許番号
US04417049

関連ノート

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