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

HRID 1413515ノート

反応式

HRID 1413515 の反応式
[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

参加物

7

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 962Water溶媒2 回HCID 7909Methyl Isobutyl Ketone溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-ebf4414391ec4e0b8bce4f4df845a77b
出典データセット
uspto-grants-1981_02
特許番号
US04250176

反応ノート

読み込み中…