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Water → HCID 68899861、化合物

HRID 735375
ノート
印刷プレビュー

反応式

HRID 735375 の反応式
[H-].C([Al+]CC(C)C)C(C)C.[F:11][C:12]1[CH:13]=[CH:14][C:15]([C:20]2[CH:29]=[CH:28][C:27]3[C:22](=[CH:23][CH:24]=[C:25]([S:30]([C:33]4[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=4)(=[O:32])=[O:31])[CH:26]=3)[CH:21]=2)=[C:16]([CH:19]=1)[C:17]#N.[BH4-].[Na+].[OH2:41]>ClCCl.CO>[F:11][C:12]1[CH:13]=[CH:14][C:15]([C:20]2[CH:29]=[CH:28][C:27]3[C:22](=[CH:23][CH:24]=[C:25]([S:30]([C:33]4[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=4)(=[O:32])=[O:31])[CH:26]=3)[CH:21]=2)=[C:16]([CH2:17][OH:41])[CH:19]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 962WaterHCID 4311764Sodium borohydrideHCID 21225700DiisobutylaluminumhydrideHCID 68900138HCID 68900138、化合物

生成物 1

HCID 68899861HCID 68899861、化合物収率 46%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒
HCID 6344
Dichloromethane
溶媒

反応条件

温度
0 °C

実験手順

A solution of diisobutylaluminium hydride (1M in dichloromethane, 700 μL, 0.70 mmol) was added to 5-fluoro-2-[6-(phenylsulfonyl)-2-naphthyl]benzonitrile (66 mg, 0.17 mmol) in dichloromethane (2 mL) at −78° C. under nitrogen and allowed to warm to 0° C. during 2 hours. It was quenched with ammonium chloride (3 mL), diluted with water (75 mL) and extracted into ethyl acetate (2×50 mL). These extracts were washed with water and brine then dried (MgSO4), filtered and solvent removed in vacuo to give the crude aldehyde as a foam. This foam (67 mg, 0.17 mmol) was suspended in methanol (4 mL) at 0° C. under nitrogen and sodium borohydride (35 mg, 0.92 mmol) added. It was stirred at this temperature for 30 minutes then allowed to return to ambient temperature over 30 minutes. Water (100 mL) was added and the mixture extracted with ethyl acetate (3×30 mL). These extracts were washed with water and brine then dried (MgSO4), filtered and solvent removed in vacuo. Purification by flash column chromatography eluting with a 10-40% ethyl acetate/isohexane gradient gave {5-fluoro-2-[6-(phenylsulfonyl)-2-naphthyl]phenyl}methanol (31 mg, 46%). 1H NMR (500 MHz, CDCl3) δ 8.62 (1H, s), 8.03-8.01 (3H, m), 7.94 (1H, d, J=8.6 Hz), 7.90 (1H, dd, J=1.7, 8.7 Hz), 7.82 (1H, s), 7.60-7.50 (4H, m), 7.35 (1H, dd, J=2.5, 9.6 Hz), 7.29 (1H, dd, J=5.6, 8.4 Hz), 7.11-7.05 (1H, m), 4.60 (2H, d, J=5.1 Hz), 1.67 (1H, t, J=5.5 Hz); m/z (ES+) 393 [MH+].

後処理

  1. customIt was quenched with ammonium chloride (3 mL)
  2. additiondiluted with water (75 mL)
  3. extractionextracted into ethyl acetate (2×50 mL)
  4. washThese extracts were washed with water and brine
  5. dry with materialthen dried (MgSO4)
  6. filtrationfiltered
  7. customsolvent removed in vacuo
  8. customto give the crude aldehyde as a foam
  9. waitto return to ambient temperature over 30 minutes
  10. extractionthe mixture extracted with ethyl acetate (3×30 mL)
  11. washThese extracts were washed with water and brine
  12. dry with materialthen dried (MgSO4)
  13. filtrationfiltered
  14. customsolvent removed in vacuo
  15. customPurification by flash column chromatography
  16. washeluting with a 10-40% ethyl acetate/isohexane gradient

出典と根拠

ORDレコード
ord-ac622db38891427295e607e76856be9d
出典データセット
uspto-grants-2009_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07592456B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート