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Water → HCID 68899861, Verbindung

HRID 735375
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 735375
[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
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

7

Edukt 4

HCID 962WaterHCID 4311764Sodium borohydrideHCID 21225700DiisobutylaluminumhydrideHCID 68900138HCID 68900138, Verbindung

Produkt 1

HCID 68899861HCID 68899861, VerbindungAusbeute 46 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 887
Methanol
Lösungsmittel
HCID 6344DichloromethaneLösungsmittel

Reaktionsbedingungen

Temperatur
0 °C

Versuchsvorschrift

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+].

Aufarbeitung

  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

Quellen und Nachweise

ORD-Eintrag
ord-ac622db38891427295e607e76856be9d
Quelldatensatz
uspto-grants-2009_09
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07592456B2

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