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Benzaldehyde → HCID 21099482、化合物

HRID 1351668
ノート
印刷プレビュー

反応式

HRID 1351668 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 3

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

生成物 1

HCID 21099482HCID 21099482、化合物収率 68%

試薬・触媒・溶媒 3

HCID 178419074HCID 178419074、化合物触媒
HCID 6344
Dichloromethane
溶媒
HCID 8857Ethyl Acetate溶媒

実験手順

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+].

後処理

  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

出典と根拠

ORDレコード
ord-b671aaa6cd0e4da6afd9511b87433aa9
出典データセット
uspto-grants-2007_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07217740B2

反応ノート

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