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

HRID 1489152노트

반응식

HRID 1489152 반응식
[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

참가 물질

6

반응물 3

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

생성물 1

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

시약·촉매·용매 2

HCID 702Ethanol용매HCID 8857Ethyl Acetate용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-542bd7980204498e812331bb63cc3354
출처 데이터셋
uspto-grants-1997_10
특허 번호
US05677326

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