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Tetrahydrofuran → 1-(1-(4-(4-Fluorophenyl)-4-hydroxybutyl)-4-piperidinyl)-1,3-dihydro-2H-benzimidazol-2-one

HRID 1578391
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HRID 1578391 반응식
[H-].[Al+3].[Li+].[H-].[H-].[H-].O1CCCC1.[F:12][C:13]1[CH:40]=[CH:39][C:16]([C:17]([CH2:19][CH2:20][C:21]([N:23]2[CH2:28][CH2:27][CH:26]([N:29]3[C:33]4[CH:34]=[CH:35][CH:36]=[CH:37][C:32]=4[NH:31][C:30]3=[O:38])[CH2:25][CH2:24]2)=O)=[O:18])=[CH:15][CH:14]=1>O>[F:12][C:13]1[CH:40]=[CH:39][C:16]([CH:17]([OH:18])[CH2:19][CH2:20][CH2:21][N:23]2[CH2:28][CH2:27][CH:26]([N:29]3[C:33]4[CH:34]=[CH:35][CH:36]=[CH:37][C:32]=4[NH:31][C:30]3=[O:38])[CH2:25][CH2:24]2)=[CH:15][CH:14]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 8028TetrahydrofuranHCID 21226445Aluminium lithium hydrideHCID 21559997HCID 21559997, 화합물

생성물 1

HCID 1937061-(1-(4-(4-Fluorophenyl)-4-hydroxybutyl)-4-piperidinyl)-1,3-dihydro-2H-benzimidazol-2-one

시약·촉매·용매 1

HCID 962Water용매

실험 절차

To a stirred mixture of 2.0 g of lithium aluminum hydride and 180 ml of tetrahydrofuran at room temperature, was added 4.6 g of 1-[1-(β-p-fluorobenzoylpropionyl)-4-piperidyl]-2-oxobenzimidazoline portionwise over a period of about 10 minutes. The mixture was further stirred at room temperature for one hour, then gradually heated to 60°C over a period of one hour, stirred for additional 4 hours at 60° - 65°C, and then cooled in ice. To the reaction mixture was carefully added 20 milliliters of cold water, and the precipitate formed was filtered off. The filtrate was added with 6 ml of acetic acid, and the tetrahydrofuran was removed by distillation under reduced pressure. The residue was made slightly alkaline by adding a 14% aqueous ammonia, and the solid precipitated was collected by filtration, dried, and recrystallized from toluene to obtain a white crystalline powder of 1-(p-fluorophenyl)-4-[4-(2-oxo-1-benzimidazolinyl)-piperidino]-1-butanol, melting at 160° - 161° C.

후처리

  1. temperaturegradually heated to 60°C over a period of one hour
  2. stirringstirred for additional 4 hours at 60° - 65°C
  3. temperaturecooled in ice
  4. customthe precipitate formed
  5. filtrationwas filtered off
  6. additionThe filtrate was added with 6 ml of acetic acid
  7. customthe tetrahydrofuran was removed by distillation under reduced pressure
  8. additionby adding a 14% aqueous ammonia
  9. customthe solid precipitated
  10. filtrationwas collected by filtration
  11. customdried
  12. customrecrystallized from toluene

출처 및 근거

ORD 기록
ord-43a160b2a7b54e77806b4b82139d292c
출처 데이터셋
uspto-grants-1976_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03936468

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