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Imidazole → 4-Chloro-α-[[[(1,1-dimethylethyl)dimethylsilyl]oxy]methyl]benzeneacetonitrile

HRID 625072
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HRID 625072 반응식
[Si:1](Cl)([C:4]([CH3:7])([CH3:6])[CH3:5])([CH3:3])[CH3:2].[Cl:9][C:10]1[CH:15]=[CH:14][C:13]([CH:16]([CH2:19][OH:20])[C:17]#[N:18])=[CH:12][CH:11]=1.N1C=CN=C1>CN(C=O)C>[Si:1]([O:20][CH2:19][CH:16]([C:13]1[CH:12]=[CH:11][C:10]([Cl:9])=[CH:15][CH:14]=1)[C:17]#[N:18])([C:4]([CH3:7])([CH3:6])[CH3:5])([CH3:3])[CH3:2]
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참가 물질

5

반응물 3

HCID 795ImidazoleHCID 28928tert-Butyldimethylsilyl chlorideHCID 66905586HCID 66905586, 화합물

생성물 1

HCID 674579324-Chloro-α-[[[(1,1-dimethylethyl)dimethylsilyl]oxy]methyl]benzeneacetonitrile수율 91%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매2회

실험 절차

TBS-Cl (2.29 g, 15.2 mmol) in dry DMF (12 mL) was added to a solution of 2-(4-chlorophenyl)-3-hydroxypropanenitrile (2.30 g, 12.7 mmol) and imidazole (3.45 g, 50.7 mmol) in DMF (20 mL) at 0° C. under nitrogen. The reaction mixture was warmed to room temperature and stirred overnight. The reaction mixture was partitioned between ether and water. The organic layer was washed with brine, dried and concentrated. The residue was purified by column (hexanes:EtOAc, 30:1) to give 3-(tert-butyldimethylsilyloxy)-2-(4-chlorophenyl)propanenitrile (3.40 g, 91%) as a colorless oil. A solution of EtMgBr in THF (3.0 M, 7.0 mL, 21 mmol) was added dropwise at room temperature to a stirred solution of this 3-(tert-butyldimethylsilyloxy)-2-(4-chlorophenyl)propanenitrile (3.1 g, 10 mmol) and Ti(i-PrO)4 (3.4 mL, 11 mmol) in Et2O (60 mL). After the mixture was stirred at room temperature for 1 hour, BF3OEt (2.7 mL, 21 mmol) was added at once. The mixture was stirred for an additional 1 hour. A solution of 10% NaOH (10 mL) was added, followed by DCM (300 mL). The resulting precipitate was filtered and washed with DCM. The combined filtrates were dried and concentrated. The residue was purified by column chromatography (30:1 DCM:MeOH) to give 1-(2-(tert-butyldimethylsilyloxy)-1-(4-chlorophenyl)ethyl)cyclopropanamine (2.3 g, 67%) as a colorless oil. LCMS: 326.1 [M+H+] (APCI+); Rf: 3.04 min.

후처리

  1. customThe reaction mixture was partitioned between ether and water
  2. washThe organic layer was washed with brine
  3. customdried
  4. concentrationconcentrated
  5. customThe residue was purified by column (hexanes:EtOAc, 30:1)

출처 및 근거

ORD 기록
ord-c55ec0d0aed344f484e1daf8554bdba2
출처 데이터셋
uspto-grants-2016_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09303040B2

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