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Hydrochloric Acid → 9-[2-HYDROXY-2-(4-METHOXYPHENYL)ETHYL]-2,3-DIHYDROIMIDAZO[1,2-a]BENZIMIDAZOLE HYDROCHLORIDE

HRID 1683732
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HRID 1683732 반응식
[BH4-].[Na+].[CH3:3][O:4][C:5]1[CH:25]=[CH:24][C:8]([C:9](=[O:23])[CH2:10][N:11]2[C:15]3[CH:16]=[CH:17][CH:18]=[CH:19][C:14]=3[N:13]3[CH2:20][CH2:21][N:22]=[C:12]23)=[CH:7][CH:6]=1.[ClH:26]>CO>[ClH:26].[OH:23][CH:9]([C:8]1[CH:7]=[CH:6][C:5]([O:4][CH3:3])=[CH:25][CH:24]=1)[CH2:10][N:11]1[C:15]2[CH:16]=[CH:17][CH:18]=[CH:19][C:14]=2[N:13]2[CH2:20][CH2:21][N:22]=[C:12]12
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참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 34790182-(2,3-dihydro-9H-imidazo[1,2-a]benzimidazol-9-yl)-1-(4-methoxyphenyl)ethanoneHCID 4311764Sodium borohydride

생성물 1

HCID 190408669-[2-HYDROXY-2-(4-METHOXYPHENYL)ETHYL]-2,3-DIHYDROIMIDAZO[1,2-a]BENZIMIDAZOLE HYDROCHLORIDE

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

Add 0.3 g (7.5 mmol) of sodium borohydride bit by bit to a suspension of 2.41 g (7 mmol) of 9-(4'-methoxyphenacyl)-2,3-dihydroimidazo[1,2-a]benzimidazole--described in Example 6--in 15 ml of methanol over a period of thirty minutes at room temperature. Continue stirring for a further four hours and leave until the next day. Subsequently, add 10 ml of 10% hydrochloric acid until a pH of 2-3 is obtained, and evaporate the methanol. Treat the residue with an ammonium hydroxide solution and extract with chloroform. Recrystallise the residue. The title compound is obtained in the form of a base. Dissolve in hot ethanol and add ethereal hydrogen chloride. Allow to cool, suction-filter, and wash with ether. The title compound is obtained.

후처리

  1. customleave until the next day
  2. customis obtained
  3. customevaporate the methanol
  4. additionTreat the residue with an ammonium hydroxide solution
  5. extractionextract with chloroform
  6. customRecrystallise the residue

출처 및 근거

ORD 기록
ord-e20d93f9b5f841128137c30ea3c135cd
출처 데이터셋
uspto-grants-1997_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05639756

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