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2-(Di-tert-butylphosphino)biphenyl → HCID 86618692, 화합물

HRID 2239366
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HRID 2239366 반응식
Br[C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([CH2:8][O:9][Si:10]([C:13]([CH3:16])([CH3:15])[CH3:14])([CH3:12])[CH3:11])[N:3]=1.[OH:17][CH2:18][C@@H:19]1[CH2:24][CH2:23][CH2:22][CH2:21][N:20]1[C:25]([O:27][C:28]([CH3:31])([CH3:30])[CH3:29])=[O:26].C(P(C(C)(C)C)C1C=CC=CC=1C1C=CC=CC=1)(C)(C)C>C1(C)C=CC=CC=1.CC([O-])=O.CC([O-])=O.[Pd+2]>[Si:10]([O:9][CH2:8][C:4]1[N:3]=[C:2]([O:17][CH2:18][C@@H:19]2[CH2:24][CH2:23][CH2:22][CH2:21][N:20]2[C:25]([O:27][C:28]([CH3:31])([CH3:30])[CH3:29])=[O:26])[CH:7]=[CH:6][CH:5]=1)([C:13]([CH3:16])([CH3:15])[CH3:14])([CH3:12])[CH3:11]
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참가 물질

6

반응물 3

HCID 27342152-(Di-tert-butylphosphino)biphenylHCID 6933954tert-Butyl (2S)-2-(hydroxymethyl)piperidine-1-carboxylateHCID 11483477Pyridine, 2-bromo-6-[[[(1,1-dimethylethyl)dimethylsilyl]oxy]methyl]-

생성물 1

HCID 86618692HCID 86618692, 화합물

시약·촉매·용매 2

HCID 167845palladium(II) acetate촉매
HCID 1140
Toluene
용매

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온도
100 °C

실험 절차

2-Bromo-6-({[tert-butyl(dimethyl)silyl]oxy}methyl)pyridine (702 mg, 2.32 mmol, from Example 21a), tert-butyl (2S)-2-(hydroxymethyl)piperidine-1-carboxylate (500 mg, 2.32 mmol), Pd(OAc)2 (26 mg, 0.116 mmol), 2-(di-t-butylphosphino)biphenyl (42 mg, 0.139 mmol) and Cs2(CO3) (1.51 g, 4.64 mmol) were mixed in toluene (20 ml). The reaction was stirred under an N2 atmosphere and heated to 100° C. on an oil bath for 24 h. The solvent was evaporated in vacuo and the residue separated between EtOAc (250 ml) and water (250 ml). The organic phase washed with water (250 ml) and the combined aqueous phases were extracted with EtOAc (250 ml). The combined EtOAc phases were dried over Na2SO4 (s), filtered and evaporated in vacuo. Purification by silica gel flash chromatography using a 40+M Biotage column with a gradient of 5-20% EtOAc in heptane yielded the title compound as a colorless oil. Yield: 729 mg (72%). 1H NMR (400 MHz, CDCl3) δ 7.43 (t, 1H, J=7.8 Hz), 6.91 (d, 1H, J=7.3 Hz), 6.44 (d, 1H, J=8.2 Hz), 4.57 (s, 2H), 4.48 (m, 1H), 4.25 (d, 2H, J=7.4 Hz), 3.91 (d, 1H, J=11.6 Hz), 2.76 (dt, 1H, J=13.3 Hz, J=2.0 Hz), 1.69 (d, 1H, J=12.0 Hz), 1.57-1.37 (m, 5H), 1.27 (s, 9H), 0.84 (s, 9H), 0.00 (s, 6H).

후처리

  1. customThe solvent was evaporated in vacuo
  2. customthe residue separated between EtOAc (250 ml) and water (250 ml)
  3. washThe organic phase washed with water (250 ml)
  4. extractionthe combined aqueous phases were extracted with EtOAc (250 ml)
  5. dry with materialThe combined EtOAc phases were dried over Na2SO4 (s)
  6. filtrationfiltered
  7. customevaporated in vacuo
  8. customPurification by silica gel flash chromatography

출처 및 근거

ORD 기록
ord-7af6daadb4a7450796743dbaa0b865ed
출처 데이터셋
uspto-grants-2010_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07723331B2

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