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Water → HCID 21099479、化合物

HRID 1351693
ノート
印刷プレビュー

反応式

HRID 1351693 の反応式
F[C:2]1[CH:7]=[C:6]([F:8])[CH:5]=[CH:4][C:3]=1/[CH:9]=[CH:10]/[C:11]1[CH:16]=[CH:15][C:14]([S:17]([C:20]2[CH:27]=[CH:26][CH:25]=[CH:24][C:21]=2[CH:22]=O)(=[O:19])=[O:18])=[CH:13][CH:12]=1.[CH3:28][C:29]([S:32]([NH2:34])=[O:33])([CH3:31])[CH3:30].[BH4-].[Na+].O>O1CCCC1.[O-]CC.[Ti+4].[O-]CC.[O-]CC.[O-]CC.ClCCl>[CH3:28][C:29]([S:32]([NH:34][CH2:22][C:21]1[CH:24]=[CH:25][CH:26]=[CH:27][C:20]=1[S:17]([C:14]1[CH:13]=[CH:12][C:11](/[CH:10]=[CH:9]/[C:3]2[CH:4]=[CH:5][C:6]([F:8])=[CH:7][CH:2]=2)=[CH:16][CH:15]=1)(=[O:18])=[O:19])=[O:33])([CH3:31])[CH3:30]
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 962WaterHCID 3382465Tert-ButanesulfinamideHCID 4311764Sodium borohydrideHCID 21099432HCID 21099432、化合物

生成物 1

HCID 21099479HCID 21099479、化合物

試薬・触媒・溶媒 3

HCID 76524Titanium tetraethoxide触媒
HCID 6344
Dichloromethane
溶媒
HCID 8028Tetrahydrofuran溶媒

実験手順

A mixture of 2-({4-[(E)-2-(2,4-difluorophenyl)vinyl]phenyl}sulfonyl)benzaldehyde (Example 176, 500 mg, 1.44 mmol), 2-methyl-2-propanesulfinamide (192 mg, 1.58 mmol) and titanium(IV) ethoxide (0.6 mL, 2.88 mmol) in tetrahydrofuran (7 mL) was heated to reflux for 4 hours. The cooled reaction mixture was partitioned between ethyl acetate and brine. The organic layer was dried over MgSO4 and evaporated in vacuo. The residue was taken up in methanol/dichloromethane (3:1, 16 mL) and sodium borohydride (424 mg, 8.64 mmol) added portionwise. After stirring at room temperature for 10 minutes, water and dichloromethane were added. The organic layer was dried over MgSO4 and concentrated in vacuo. The residue was purified by flash column chromatography on silica, eluting with 50–90% ethyl acetate/isohexane, followed by recrystallisation to give the title compound as a white solid. δH (500 MHz, d6 DMSO): 8.11 (1H, d, J=7.8 Hz), 7.84–7.80 (4H, m), 7.73–7.66 (4H, m), 7.59–7.57 (1H, m), 7.45 (1H, d, J=16.4 Hz), 7.30 (1H, d, J=16.5 Hz), 7.23 (2H, t, J=8.8 Hz), 5.78 (1H, t, J=6.4 Hz), 4.45–4.35 (2H, m), 1.07 (9H, s).

後処理

  1. temperaturewas heated
  2. temperatureto reflux for 4 hours
  3. customThe cooled reaction mixture
  4. customwas partitioned between ethyl acetate and brine
  5. dry with materialThe organic layer was dried over MgSO4
  6. customevaporated in vacuo
  7. dry with materialThe organic layer was dried over MgSO4
  8. concentrationconcentrated in vacuo
  9. customThe residue was purified by flash column chromatography on silica
  10. washeluting with 50–90% ethyl acetate/isohexane
  11. customfollowed by recrystallisation

出典と根拠

ORDレコード
ord-cc6c866be6e54ff9954ff9947becbf50
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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