Potassium Iodide → 5-[4-(diphenylmethyl)-1-piperazinyl]pentyl-1,3-dihydro-2H-benzimidazol-2-one dihydrochloride

HRID 1413515노트

반응식

HRID 1413515 반응식
[Cl:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][N:7]1[C:11]2[CH:12]=[CH:13][CH:14]=[CH:15][C:10]=2[N:9](C(C)=C)[C:8]1=[O:19].[C:20]1([CH:26]([C:33]2[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=2)[N:27]2[CH2:32][CH2:31][NH:30][CH2:29][CH2:28]2)[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1.C(=O)([O-])[O-].[Na+].[Na+].[I-].[K+]>O.CC(C)CC(=O)C>[ClH:1].[ClH:1].[C:33]1([CH:26]([C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)[N:27]2[CH2:28][CH2:29][N:30]([CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][N:7]3[C:11]4[CH:12]=[CH:13][CH:14]=[CH:15][C:10]=4[NH:9][C:8]3=[O:19])[CH2:31][CH2:32]2)[CH:34]=[CH:35][CH:36]=[CH:37][CH:38]=1

참가 물질

7

반응물 4

HCID 4875Potassium IodideHCID 10340Sodium CarbonateHCID 70048BenzhydrylpiperazineHCID 205063661-(5-chloropentyl)-1,3-dihydro-3-(1-methylethenyl)-2H-benzimidazol-2-one

생성물 1

HCID 867374905-[4-(diphenylmethyl)-1-piperazinyl]pentyl-1,3-dihydro-2H-benzimidazol-2-one dihydrochloride

시약·촉매·용매 2

HCID 962Water용매2회HCID 7909Methyl Isobutyl Ketone용매

실험 절차

A mixture of 6.95 parts of 1-(5-chloropentyl)-1,3-dihydro-3-(1-methylethenyl)-2H-benzimidazol-2-one, 5.15 parts of 1-(diphenylmethyl)piperazine, 5.30 parts of sodium carbonate, 0.1 parts of potassium iodide and 160 parts of 4-methyl-2-pentanone is stirred and refluxed overnight with water-separator. The reaction mixture is cooled to room temperature, water is added and the layers are separated. The organic phase is dried filtered and evaporated. The residue is stirred and refluxed for 30 minutes with 12 parts of a hydrochloric acid solution in 40 parts of ethanol. The whole is evaporated and the residue is crystallized from ethanol, yielding 1-{5-[4-(diphenylmethyl)-1-piperazinyl]pentyl-1,3-dihydro-2H-benzimidazol-2-one dihydrochloride.hydrate; mp. 215.3° C.

후처리

  1. customthe layers are separated
  2. customThe organic phase is dried
  3. filtrationfiltered
  4. customevaporated
  5. stirringThe residue is stirred
  6. temperaturerefluxed for 30 minutes with 12 parts of a hydrochloric acid solution in 40 parts of ethanol
  7. customThe whole is evaporated
  8. customthe residue is crystallized from ethanol

출처 및 근거

ORD 기록
ord-ebf4414391ec4e0b8bce4f4df845a77b
출처 데이터셋
uspto-grants-1981_02
특허 번호
US04250176

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