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Benzaldehyde → HCID 21099482, 화합물

HRID 1351668
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HRID 1351668 반응식
[F:1][C:2]1[CH:7]=[C:6]([F:8])[CH:5]=[CH:4][C:3]=1[CH2:9][CH2:10][C:11]1[CH:16]=[CH:15][C:14]([S:17]([C:20]2[CH:21]=[C:22]([CH2:26][OH:27])[CH:23]=[CH:24][CH:25]=2)(=[O:19])=[O:18])=[CH:13][CH:12]=1.C(=O)C1C=CC=CC=1.C[N+]1([O-])CCOCC1>ClCCl.C(OCC)(=O)C.[Ru]([O-])(=O)(=O)=O.C([N+](CCC)(CCC)CCC)CC>[F:1][C:2]1[CH:7]=[C:6]([F:8])[CH:5]=[CH:4][C:3]=1[CH2:9][CH2:10][C:11]1[CH:12]=[CH:13][C:14]([S:17]([C:20]2[CH:21]=[C:22]([CH:23]=[CH:24][CH:25]=2)[CH:26]=[O:27])(=[O:18])=[O:19])=[CH:15][CH:16]=1
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참가 물질

7

반응물 3

HCID 240BenzaldehydeHCID 82029Methyl morpholine oxideHCID 21099483[3-({4-[2-(2,4-Difluorophenyl)ethyl]phenyl]sulfonyl)phenyl]methanol

생성물 1

HCID 21099482HCID 21099482, 화합물수율 68%

시약·촉매·용매 3

HCID 178419074HCID 178419074, 화합물촉매
HCID 6344
Dichloromethane
용매
HCID 8857Ethyl Acetate용매

실험 절차

To a solution of [3-({4-[2-(2,4-difluorophenyl)ethyl]phenyl}sulfonyl)phenyl]methanol (prepared from 3-({4-[E)-2-(2,4-difluorophenyl)vinyl]phenyl}sulfonyl)benzaldehyde (Example 50 Step 1) according to the method of Example 117) in dichloromethane (4 mL) was added 4 Å molecular sieves (0.1 g) and the mixture stirred for 10 minutes. 4-Methylmorpholine N-oxide (68 mg, 0.58 mmol) was added in one portion and the reaction stirred for 10 minutes, then tetrapropylammonium perruthenate (6.9 mg, 0.02 mmol) added. The reaction was stirred for 30 minutes then diluted with ethyl acetate, filtered through a pad of silica and washed with further ethyl acetate. The filtrate was evaporated in vacuo. The residue was purified by flash column chromatography on silica, eluting with 25% ethyl acetate/isohexane, to yield 3-({4-[2-(2,4-difluorophenyl)ethyl]phenyl}sulfonyl)benzaldehyde (103 mg, 68%). δH (400 MHz, CDCl3): 10.06 (1H, s), 8.40 (1H, s), 8.18 (1H, d, J=7.8 Hz), 8.07 (1H, d, J=7.6 Hz), 7.87 (2H, d, J=8.3 Hz), 7.69 (1H, t, J=7.7 Hz), 7.30 (2H, d, J=8.2 Hz), 6.99 (1H, q, J=7.9 Hz), 6.79–6.73 (2H, m), 2.95–2.87 (4H, m). m/z ES+) 387 [MH+].

후처리

  1. additionwas added 4 Å molecular sieves (0.1 g)
  2. stirringthe reaction stirred for 10 minutes
  3. stirringThe reaction was stirred for 30 minutes
  4. filtrationfiltered through a pad of silica
  5. washwashed with further ethyl acetate
  6. customThe filtrate was evaporated in vacuo
  7. customThe residue was purified by flash column chromatography on silica
  8. washeluting with 25% ethyl acetate/isohexane

출처 및 근거

ORD 기록
ord-b671aaa6cd0e4da6afd9511b87433aa9
출처 데이터셋
uspto-grants-2007_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07217740B2

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