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1,2-Dichloroethane → 2-{[(4-Fluorophenyl)methyl]oxy}-N-4-isoxazolyl-5-(1-methyl-1H-pyrazol-4-yl)benzamide

HRID 1623871
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HRID 1623871 반응식
[F:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][O:9][C:10]2[CH:18]=[CH:17][C:16]([C:19]3[CH:20]=[N:21][N:22]([CH3:24])[CH:23]=3)=[CH:15][C:11]=2[C:12](O)=[O:13])=[CH:4][CH:3]=1.[O:25]1[CH:29]=[C:28]([NH2:30])[CH:27]=[N:26]1.C1C=CC2N(O)N=NC=2C=1.C(Cl)CCl>CN(C)C=O.O>[F:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][O:9][C:10]2[CH:18]=[CH:17][C:16]([C:19]3[CH:20]=[N:21][N:22]([CH3:24])[CH:23]=3)=[CH:15][C:11]=2[C:12]([NH:30][C:28]2[CH:27]=[N:26][O:25][CH:29]=2)=[O:13])=[CH:4][CH:3]=1
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참가 물질

7

반응물 4

HCID 111,2-DichloroethaneHCID 757711-HydroxybenzotriazoleHCID 138042781,2-Oxazol-4-amineHCID 67108246HCID 67108246, 화합물

생성물 1

HCID 699368062-{[(4-Fluorophenyl)methyl]oxy}-N-4-isoxazolyl-5-(1-methyl-1H-pyrazol-4-yl)benzamide

시약·촉매·용매 2

HCID 962Water
용매
HCID 6228Dimethylformamide용매

실험 절차

A mixture of 2-{[(4-fluorophenyl)methyl]oxy}-5-(1-methyl-1H-pyrazol-4-yl)benzoic acid (may be prepared as described in Description 121; 100 mg, 0.31 mmol), isoxazol-4-amine (38.6 mg, 0.46 mmol), HOBT (70.4 mg, 0.46 mmol) and EDC (88 mg, 0.46 mmol) in N,N-dimethylformamide (5 ml) was stirred at room temperature for 16 hours. Water (50 ml) was added. The mixture was extracted with ethyl acetate (50 ml×3). The combined organic layers were washed with brine (50 ml), dried over Na2SO4, and concentrated to give the crude product. The crude product was purified by a prep-HPLC (instrument: Gilson GX-281; Column: Shimadzu PRC-ODS, 15.0 um, 19 mm*250 mm; Mobile Phase: A: 0.05% NH3H2O/H2O; B: CH3CN; Gradient 0-8 min 42-54% B; 8-12 min 95%; Flow Rate (ml/min) 30.00; Detective Wavelength (nm) 214; Retention Time (min) 7.5) to yield the title compound as a white solid. 17 mg.

후처리

  1. extractionThe mixture was extracted with ethyl acetate (50 ml×3)
  2. washThe combined organic layers were washed with brine (50 ml)
  3. dry with materialdried over Na2SO4
  4. concentrationconcentrated
  5. customto give the crude product
  6. customThe crude product was purified by a prep-HPLC (instrument
  7. customGradient 0-8 min 42-54% B
  8. custom8-12 min 95%

출처 및 근거

ORD 기록
ord-823bf75363a14ab2968c6026e3c7f727
출처 데이터셋
uspto-grants-2014_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08778939B2

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