Benzimidazole → 1-{4-[4-(2-pyrimidinyl)-1-piperazinyl]butyl}-1H-benzimidazole

HRID 483873

반응식

HRID 483873 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.[N:18]1[C:22]2[CH:23]=[CH:24][CH:25]=[CH:26][C:21]=2[NH:20][CH: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[C:22]3[CH:23]=[CH:24][CH:25]=[CH:26][C:21]=3[N:20]=[CH:19]2)[CH2:16][CH2:17]1

참가 물질

5

반응물 3

HCID 5798BenzimidazoleHCID 11430Potassium CarbonateHCID 6575058-Aza-5-azoniaspiro(4.5)decane, 8-(2-pyrimidinyl)-, bromide (1:1)

생성물 1

HCID 98191481-{4-[4-(2-pyrimidinyl)-1-piperazinyl]butyl}-1H-benzimidazole

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A mixture of 450 g (1.50 moles) of 8-(2-pyrimidinyl)-8-aza-5-azoniaspiro[4,5]decane bromide, 177 g (1.50 moles) of benzimidazole and 307 g (2.25 moles) of potassium carbonate in 2 l of dimethylformamide is heated to 140°-145° 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 457 g (91%) of 1-{4-[4-(2-pyrimidinyl)-1-piperazinyl]butyl}-1H-benzimidazole, with a melting point of 85°-88° C., are obtained.

후처리

  1. temperatureis heated to 140°-145° C. 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 457 g (91%) of 1-{4-[4-(2-pyrimidinyl)-1-piperazinyl]butyl}-1H-benzimidazole, with a melting point of 85°-88° C.
  7. customare obtained

출처 및 근거

ORD 기록
ord-7d45aa6c12ef49eeba4c69f783581040
출처 데이터셋
uspto-grants-1993_07
특허 번호
US05227486

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