Pyrazole → 1-{4-[4-(2-pyrimidinyl)-1-piperazinyl]butyl}-1H-pyrazole

HRID 483874

反応式

HRID 483874 の反応式
[Br-].[N:2]1[CH:7]=[CH:6][CH:5]=[N:4][C:3]=1[N:8]1[CH2:17][CH2:16][N+:11]2([CH2:15][CH2:14][CH2:13][CH2:12]2)[CH2:10][CH2:9]1.[NH:18]1[CH:22]=[CH:21][CH:20]=[N:19]1.C(=O)([O-])[O-].[K+].[K+]>CN(C)C=O>[N:4]1[CH:5]=[CH:6][CH:7]=[N:2][C:3]=1[N:8]1[CH2:9][CH2:10][N:11]([CH2:15][CH2:14][CH2:13][CH2:12][N:18]2[CH:22]=[CH:21][CH:20]=[N:19]2)[CH2:16][CH2:17]1

参加物

5

反応物 3

HCID 1048PyrazoleHCID 11430Potassium CarbonateHCID 6575058-Aza-5-azoniaspiro(4.5)decane, 8-(2-pyrimidinyl)-, bromide (1:1)

生成物 1

HCID 110443661-{4-[4-(2-pyrimidinyl)-1-piperazinyl]butyl}-1H-pyrazole

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
140 °C

実験手順

A mixture of 730 g (3.59 moles) of 8-(2-pyrimidinyl)-8-aza-5-azoniaspiro[4,5]decane bromide, 275 g (4.05 moles) of pyrazole and 745 g (5.4 moles) of potassium carbonate in 3 1 of dimethylformamide is heated to 140° C. for 14 hours. The mixture is evaporated under vacuum, chloroform is added, the solution is washed with water, dried over sodium sulfate and evaporated under vacuum, and 650 g (94%) of 1-{4-[4-(2-pyrimidinyl)-1-piperazinyl]butyl}-1H-pyrazole are obtained in liquid form.

後処理

  1. customThe mixture is evaporated under vacuum, chloroform
  2. additionis added
  3. washthe solution is washed with water
  4. dry with materialdried over sodium sulfate
  5. customevaporated under vacuum, and 650 g (94%) of 1-{4-[4-(2-pyrimidinyl)-1-piperazinyl]butyl}-1H-pyrazole
  6. customare obtained in liquid form

出典と根拠

ORDレコード
ord-00438c32cf89405f95ce1ee33dcba21e
出典データセット
uspto-grants-1993_07
特許番号
US05227486

関連ノート

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