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Trimethylsilyl cyanide → 2-Amino-1-[5'-isopropyl-2'-methoxy-4-(trifluoromethyl)biphenyl-2-yl]ethanol

HRID 1994489
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1994489
[CH:1]([C:4]1[CH:5]=[CH:6][C:7]([O:22][CH3:23])=[C:8]([C:10]2[C:11]([CH:20]=[O:21])=[CH:12][C:13]([C:16]([F:19])([F:18])[F:17])=[CH:14][CH:15]=2)[CH:9]=1)([CH3:3])[CH3:2].C[Si]([C:28]#[N:29])(C)C>C(Cl)Cl.[Zn+2].[I-].[I-]>[NH2:29][CH2:28][CH:20]([C:11]1[CH:12]=[C:13]([C:16]([F:17])([F:18])[F:19])[CH:14]=[CH:15][C:10]=1[C:8]1[CH:9]=[C:4]([CH:1]([CH3:3])[CH3:2])[CH:5]=[CH:6][C:7]=1[O:22][CH3:23])[OH:21]
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Komponenten

5

Edukt 2

HCID 82115Trimethylsilyl cyanideHCID 578779885'-Isopropyl-2'-methoxy-4-(trifluoromethyl)biphenyl-2-carbaldehyde

Produkt 1

HCID 667170952-Amino-1-[5'-isopropyl-2'-methoxy-4-(trifluoromethyl)biphenyl-2-yl]ethanol

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 9883512zinc(II)iodideKatalysatorHCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

To a solution of 0.679 g of 5′-isopropyl-2′-methoxy-4-(trifluoromethyl)biphenyl-2-carbaldehyde in 1.5 mL of CH2Cl2 was added ca. 5 mg of ZnI2, then 0.23 g of trimethylsilyl cyanide. The mixture was stirred at room temperature for 3 h, and then partitioned between 15 mL of water and 10 mL of Et2O. The aqueous phase was extracted with 2×10 mL of Et2O. The combined organics were dried over Na2SO4 and concentrated. The residue was dissolved in 15 mL of Et2O and cooled to 0° C. A 1-M solution of LiAlH4 in Et2O (4.2 mL) was added dropwise via addition funnel. The cooling bath was removed once the addition was complete, and the mixture was stirred overnight at room temperature, then recooled to 0° C. and quenched by dropwise addition of 0.15 mL of water, 0.15 mL of 15% aqueous NaOH, and 0.4 mL of water. The cooling bath was removed once the addition was complete, and the mixture was stirred 30 min at room temperature, filtered (washing the solids liberally with Et2O), and concentrated to provide the title compound, which was used without further purification. Mass spectrum (ESI) 354.2 (M+1). Some 1H NMR signals are doubled because of atropoisomerism. 1H NMR (500 MHz, CDCl3): δ 7.88 (s, 1H), 7.55 (app t, J=7.5 Hz, 1H), 7.22-7.28 (m, 2H), 6.99, 6.95 (d, J=2.5 Hz, 1H), 6.92, 6.90 (sm 1H), 4.52 (m, 1H), 3.70 (s, 3H), 2.90 (septet, J=7 Hz, 1H), 2.81 (m, 1H), 2.60-2.70 (m, 2H), 1.23-1.28 (m, 6H).

Aufarbeitung

  1. custompartitioned between 15 mL of water and 10 mL of Et2O
  2. extractionThe aqueous phase was extracted with 2×10 mL of Et2O
  3. dry with materialThe combined organics were dried over Na2SO4
  4. concentrationconcentrated
  5. dissolutionThe residue was dissolved in 15 mL of Et2O
  6. temperaturecooled to 0° C
  7. additionA 1-M solution of LiAlH4 in Et2O (4.2 mL) was added dropwise via addition funnel
  8. customThe cooling bath was removed once the addition
  9. stirringthe mixture was stirred overnight at room temperature
  10. customrecooled to 0° C.
  11. customquenched by dropwise addition of 0.15 mL of water, 0.15 mL of 15% aqueous NaOH, and 0.4 mL of water
  12. customThe cooling bath was removed once the addition
  13. stirringthe mixture was stirred 30 min at room temperature
  14. filtrationfiltered (
  15. washwashing the solids liberally with Et2O), and
  16. concentrationconcentrated

Quellen und Nachweise

ORD-Eintrag
ord-fab7dc20f2544b68bef3cb0af0e08619
Quelldatensatz
uspto-grants-2010_01
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07652049B2

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