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

HRID 483872

반응식

HRID 483872 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-a16ab31c82c946d3aceec834d8713024
출처 데이터셋
uspto-grants-1993_07
특허 번호
US05227486

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