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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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HRID 1994489 반응식
[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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참가 물질

5

반응물 2

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

생성물 1

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

시약·촉매·용매 2

HCID 9883512zinc(II)iodide촉매HCID 6344Dichloromethane용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-fab7dc20f2544b68bef3cb0af0e08619
출처 데이터셋
uspto-grants-2010_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07652049B2

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