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Dimethyl Sulfoxide → 4-[1-Benzyl-4-(3-methoxy-phenyl)-piperidin-4-yl]-benzoic acid methyl ester

HRID 2085455
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HRID 2085455 반응식
[CH2:1]([N:8]1[CH2:13][CH2:12][C:11]([C:22]2[CH:27]=[CH:26][C:25](OS(C(F)(F)F)(=O)=O)=[CH:24][CH:23]=2)([C:14]2[CH:19]=[CH:18][CH:17]=[C:16]([O:20][CH3:21])[CH:15]=2)[CH2:10][CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.CS(C)=[O:38].C(N(CC)CC)C.C1(P(C2C=CC=CC=2)CCCP(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.[CH2:76]([O:78][CH2:79]C)C>CO.C([O-])(=O)C.[Pd+2].C([O-])(=O)C>[CH3:76][O:78][C:79](=[O:38])[C:25]1[CH:24]=[CH:23][C:22]([C:11]2([C:14]3[CH:19]=[CH:18][CH:17]=[C:16]([O:20][CH3:21])[CH:15]=3)[CH2:12][CH2:13][N:8]([CH2:1][C:2]3[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=3)[CH2:9][CH2:10]2)=[CH:27][CH:26]=1
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참가 물질

8

반응물 5

HCID 679Dimethyl SulfoxideHCID 3283Diethyl EtherHCID 8471TriethylamineHCID 812191,3-Bis(diphenylphosphino)propaneHCID 54436264Trifluoro-methanesulfonic acid 4-[1-benzyl-4-(3-methoxy-phenyl)piperidin-4-yl]-phenyl ester

생성물 1

HCID 53835840
4-[1-Benzyl-4-(3-methoxy-phenyl)-piperidin-4-yl]-benzoic acid methyl ester
수율 85%

시약·촉매·용매 2

HCID 167845palladium(II) acetate촉매HCID 887Methanol용매

반응 조건

온도
70 °C

실험 절차

To a solution of trifluoro-methanesulfonic acid 4-[1-benzyl-4-(3-methoxy-phenyl)-piperidin-4-yl]-phenyl ester (10.0 g, 19.8 mmol) in a Parr pressure bottle in MeOH (69 mL) were added DMSO (62 mL) and triethylamine (21.8 mL, 157 mmol). To the reaction mixture were added palladium acetate (2.2 g, 9.1 mmol) and 1,3-bis(diphenylphosphino)propane (3.75 g, 9.1 mmol). The mixture was shaken under 40 psi of CO at 70° C. for 4 hours. The reaction mixture was cooled to room temperature and was diluted with diethyl ether (600 mL). The ether layer was washed with water (5×60 mL), dried (MgSO4) and concentrated. The crude residue was purified by flash chromatography with hexanes/EtOAc (1:1) to afford 6.9 g (85% yield) of 4-[1-Benzyl-4-(3-methoxy-phenyl)-piperidin-4-yl]-benzoic acid methyl ester. 1HNMR (400 MHz, CDCl3) δ 7.91 (d, 2H), 7.32 (d, 2H), 7.28-7.16 (comp, 6H),), 6.82 (d, , 1H), 6.79 (s, 1H), 6.68 (dd, 1H), 3.86 (s, 3H), 3.74 (s, 3H), 3.38 (s, 2H), 2.47-2.44 (comp, 8H); MS (M+1) 416.2.

후처리

  1. temperatureThe reaction mixture was cooled to room temperature
  2. washThe ether layer was washed with water (5×60 mL)
  3. dry with materialdried (MgSO4)
  4. concentrationconcentrated
  5. customThe crude residue was purified by flash chromatography with hexanes/EtOAc (1:1)

출처 및 근거

ORD 기록
ord-73e49a697f9e449a8dd1348f7706770e
출처 데이터셋
uspto-grants-2004_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06720336B2

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