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Formaldehyde → 4-[(4-Chlorophenyl)sulfonyl]-4-(2,5-difluorophenyl)-1-methylpiperidine

HRID 748803
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HRID 748803 반응식
Cl.[Cl:2][C:3]1[CH:8]=[CH:7][C:6]([S:9]([C:12]2([C:18]3[CH:23]=[C:22]([F:24])[CH:21]=[CH:20][C:19]=3[F:25])[CH2:17][CH2:16][NH:15][CH2:14][CH2:13]2)(=[O:11])=[O:10])=[CH:5][CH:4]=1.[CH2:26](N(CC)CC)C.C=O.C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+].[OH-].[Na+]>C(OC(C)C)(C)C.ClCCl.C(OCC)C>[Cl:2][C:3]1[CH:8]=[CH:7][C:6]([S:9]([C:12]2([C:18]3[CH:23]=[C:22]([F:24])[CH:21]=[CH:20][C:19]=3[F:25])[CH2:17][CH2:16][N:15]([CH3:26])[CH2:14][CH2:13]2)(=[O:10])=[O:11])=[CH:5][CH:4]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

9

반응물 5

HCID 712FormaldehydeHCID 8471TriethylamineHCID 14798Sodium HydroxideHCID 5049666Sodium triacetoxyborohydrideHCID 692029464-[(4-Chlorophenyl)sulfonyl]-4-(2,5-difluorophenyl)piperidine Hydrochloride

생성물 1

HCID 597509094-[(4-Chlorophenyl)sulfonyl]-4-(2,5-difluorophenyl)-1-methylpiperidine
수율 74%

시약·촉매·용매 3

HCID 3283Diethyl Ether용매HCID 6344Dichloromethane용매2회HCID 7914Diisopropyl Ether용매

실험 절차

To dichloromethane (5 ml) were added 4-[(4-chlorophenyl)sulfonyl]-4-(2,5-difluorophenyl)piperidine hydrochloride (100 mg, 0.245 mmol), triethylamine (0.070 ml, 0.50 mmol) and a 37% aqueous formaldehyde solution (0.060 ml, 0.739 mmol), followed by the addition of sodium triacetoxyborohydride (220 mg, 1.04 mmol) at room temperature. After stirring at room temperature for 14 hours, a 1N aqueous sodium hydroxide solution (6.0 ml) was added. The mixture was stirred at room temperature for 30 minutes. To the reaction mixture was added diethyl ether and the mixture was washed with a 1N aqueous sodium hydroxide solution. The organic layer was dried over anhydrous sodium sulfate. After filtration, the filtrate was concentrated under reduced pressure. The residue thus obtained was subjected to flash silica gel chromatography, and the fraction obtained from the dichloromethane:methanol=30:1 eluate was concentrated under reduced pressure to give a white solid. The solid thus obtained was washed with diisopropyl ether, whereby the title compound (70 mg, 0.18 mmol, 74%) was obtained as a white powder.

후처리

  1. stirringThe mixture was stirred at room temperature for 30 minutes
  2. washthe mixture was washed with a 1N aqueous sodium hydroxide solution
  3. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  4. filtrationAfter filtration
  5. concentrationthe filtrate was concentrated under reduced pressure
  6. customThe residue thus obtained
  7. concentrationmethanol=30:1 eluate was concentrated under reduced pressure
  8. customto give a white solid
  9. customThe solid thus obtained

출처 및 근거

ORD 기록
ord-d2635380630d4519a0d10fa4846b551c
출처 데이터셋
uspto-grants-2008_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07399775B2

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