Potassium Carbonate → 4,5-dichloro-2-methyl-1-(4-[4-(2-pyrimidinyl)-1-piperazinyl]butyl}-1H-imidazole

HRID 483872

反応式

HRID 483872 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.[Cl:18][C:19]1[N:20]=[C:21]([CH3:25])[NH:22][C:23]=1[Cl:24].C(=O)([O-])[O-].[K+].[K+]>CN(C)C=O>[Cl:18][C:19]1[N:20]=[C:21]([CH3:25])[N:22]([CH2:12][CH2:13][CH2:14][CH2:15][N:11]2[CH2:10][CH2:9][N:8]([C:3]3[N:2]=[CH:7][CH:6]=[CH:5][N:4]=3)[CH2:17][CH2:16]2)[C:23]=1[Cl:24]

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 3123904,5-Dichloro-2-methyl-1H-imidazoleHCID 6575058-Aza-5-azoniaspiro(4.5)decane, 8-(2-pyrimidinyl)-, bromide (1:1)

生成物 1

HCID 99292344,5-dichloro-2-methyl-1-(4-[4-(2-pyrimidinyl)-1-piperazinyl]butyl}-1H-imidazole

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A mixture of 450 g (1.5 moles) of 8-(2-pyrimidinyl)-8-aza-5-azoniaspiro[4,5]decane bromide, 225 g (1.5 moles) of 4.5-dichloro-2-methylimidazole and 300 g (2.25 moles) of potassium carbonate in 2 l of dimethylformamide is heated to 130°-135° 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 503 g (91%) of 4,5-dichloro-2-methyl-1-{4-[4-(2-pyrimidinyl)-1-piperazinyl]butyl}-1H-imidazole are obtained in liquid form.

後処理

  1. temperatureis heated to 130°-135° for 14 hours
  2. customThe mixture is evaporated under vacuum, chloroform
  3. additionis added
  4. washthe solution is washed with water
  5. dry with materialdried over sodium sulfate
  6. customevaporated under vacuum, and 503 g (91%) of 4,5-dichloro-2-methyl-1-{4-[4-(2-pyrimidinyl)-1-piperazinyl]butyl}-1H-imidazole
  7. customare obtained in liquid form

出典と根拠

ORDレコード
ord-a16ab31c82c946d3aceec834d8713024
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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