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Cyclohexanone → 4-Chloro-2-(4-cyclohexylpiperazin-1-yl)-5,7-difluoro-3-methylquinoline

HRID 1431646
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HRID 1431646 반응식
FC(F)(F)C(O)=O.[Cl:8][C:9]1[C:18]2[C:13](=[CH:14][C:15]([F:20])=[CH:16][C:17]=2[F:19])[N:12]=[C:11]([N:21]2[CH2:26][CH2:25][NH:24][CH2:23][CH2:22]2)[C:10]=1[CH3:27].C(N(CC)CC)C.[C:35]1(=O)[CH2:40][CH2:39][CH2:38][CH2:37][CH2:36]1.ClC(Cl)C.CO.C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+].C([BH3-])#N.[Na+]>C(Cl)Cl.O>[Cl:8][C:9]1[C:18]2[C:13](=[CH:14][C:15]([F:20])=[CH:16][C:17]=2[F:19])[N:12]=[C:11]([N:21]2[CH2:26][CH2:25][N:24]([CH:35]3[CH2:40][CH2:39][CH2:38][CH2:37][CH2:36]3)[CH2:23][CH2:22]2)[C:10]=1[CH3:27]
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참가 물질

9

반응물 6

HCID 7967CyclohexanoneHCID 8471TriethylamineHCID 5003444Sodium cyanoborohydride2회HCID 5049666Sodium triacetoxyborohydrideHCID 22036585Dichloroethane methanolHCID 866495114-Chloro-5,7-difluoro-3-methyl-2-(piperazin-1-yl)quinoline 2,2,2-trifluoroacetate

생성물 1

HCID 59631258
4-Chloro-2-(4-cyclohexylpiperazin-1-yl)-5,7-difluoro-3-methylquinoline

시약·촉매·용매 2

HCID 962Water용매HCID 6344Dichloromethane용매

실험 절차

The 4-chloro-5,7-difluoro-3-methyl-2-(piperazin-1-yl)quinoline 2,2,2-trifluoroacetate (75 mg, 0.18 mmol), triethylamine (0.025 mL, 0.18 mmol) and cyclohexanone (0.019 mL, 0.18 mmol) were added to 3 mL of a 2:1 dichlorethane/MeOH mixture. The sodium triacetoxyborohydride (120 mg, 0.55 mmol) was added and the slurry was stirred at rt for 4.5 h. Sodium cyanoborohydride (55 mg, 0.87 mmol) was then added and the slurry was stirred at rt for 4.5 h. Another aliquot of sodium cyanoborohydride (55 mg, 0.87 mmol) was added and the reaction was heated to 80° C. and stirred overnight. The reaction was cooled and then diluted with DCM and water. The layers were separated and the aq. layer was extracted (2×75 mL) with EtOAc. The layers were combined and washed with brine (1×50 mL) and dried over magnesium sulfate. The crude product was purified by medium pressure chromatography (silica gel, 0 to 100% EtOAc:hexanes) to give 4-chloro-2-(4-cyclohexylpiperazin-1-yl)-5,7-difluoro-3-methylquinoline. Mass Spectrum (ESI) m/e=298.1 (M+1).

후처리

  1. stirringthe slurry was stirred at rt for 4.5 h
  2. temperaturethe reaction was heated to 80° C.
  3. stirringstirred overnight
  4. temperatureThe reaction was cooled
  5. customThe layers were separated
  6. extractionthe aq. layer was extracted (2×75 mL) with EtOAc
  7. washwashed with brine (1×50 mL)
  8. dry with materialdried over magnesium sulfate
  9. customThe crude product was purified by medium pressure chromatography (silica gel, 0 to 100% EtOAc:hexanes)

출처 및 근거

ORD 기록
ord-3e2ef791a2f34b7f90e22d669ad9cc6e
출처 데이터셋
uspto-grants-2015_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08940724B2

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