Acetone → 5-[(3-Phenylindolin-1-yl)carbonyl]-4,5,6,7-tetrahydrobenzimidazole hydrochloride

HRID 1489152ノート

反応式

HRID 1489152 の反応式
[C:1]1([CH:7]2[C:15]3[C:10](=[CH:11][CH:12]=[CH:13][CH:14]=3)[N:9]([C:16]([CH:18]3[CH2:26][CH2:25][C:21]4[N:22]=[CH:23][NH:24][C:20]=4[CH2:19]3)=[O:17])[CH2:8]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[ClH:27].CC(C)=O>C(O)C.C(OCC)(=O)C>[ClH:27].[C:1]1([CH:7]2[C:15]3[C:10](=[CH:11][CH:12]=[CH:13][CH:14]=3)[N:9]([C:16]([CH:18]3[CH2:26][CH2:25][C:21]4[N:22]=[CH:23][NH:24][C:20]=4[CH2:19]3)=[O:17])[CH2:8]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

参加物

6

反応物 3

HCID 180AcetoneHCID 313Hydrochloric AcidHCID 98410295-(3-Phenylindolin-1-ylcarbonyl)-4,5,6,7-tetrahydrobenzimidazole

生成物 1

HCID 104298255-[(3-Phenylindolin-1-yl)carbonyl]-4,5,6,7-tetrahydrobenzimidazole hydrochloride

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 8857Ethyl Acetate溶媒

実験手順

A 100 mg portion of the 5-[(3-phenylindolin-1-yl)carbonyl]-4,5,6,7-tetrahydrobenzimidazole produced in the preferred embodiment 3 was dissolved in 5 ml ethanol, and 0.5 ml of a 4N hydrogen chloride solution in ethyl acetate was added under ice cooling, after which concentration under reduced pressure gave an oily residue. Five ml of acetone was added to precipitate crystals which were collected by filtration. The crystals were dissolved in 1 ml of water and then reconcentrated under reduced pressure and thoroughly dried to obtain the 5-[(3-phenylindolin-1-yl)carbonyl]-4,5,6,7-tetrahydrobenzimidazole hydrochloride (compound 4) listed in the above heading.

後処理

  1. concentrationafter which concentration under reduced pressure
  2. customgave an oily residue
  3. customto precipitate crystals which
  4. filtrationwere collected by filtration
  5. dissolutionThe crystals were dissolved in 1 ml of water
  6. customthoroughly dried

出典と根拠

ORDレコード
ord-542bd7980204498e812331bb63cc3354
出典データセット
uspto-grants-1997_10
特許番号
US05677326

反応ノート

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