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Hydroxylamine → HCID 59533941, 화합물

HRID 2167334
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HRID 2167334 반응식
[N:1]1[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[O:7][C:8]1[CH:15]=[CH:14][C:11]([C:12]#[N:13])=[CH:10][CH:9]=1.[NH2:16][OH:17]>C(O)C>[OH:17]/[N:16]=[C:12](\[NH2:13])/[C:11]1[CH:10]=[CH:9][C:8]([O:7][C:2]2[CH:3]=[CH:4][CH:5]=[CH:6][N:1]=2)=[CH:15][CH:14]=1
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HCID 787HydroxylamineHCID 185258324-(Pyridin-2-yloxy)benzonitrile

생성물 1

HCID 59533941HCID 59533941, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

4-(Pyridin-2-yloxy)benzonitrile (701 mg, 3.57 mmol) was dissolved in ethanol (14.0 mL), and hydroxylamine (472 mg, 14.3 mmol) was added and the mixture was refluxed for 16 hours. The reaction was cooled to room temperature and then concentrated in vacuo to give the product as a yellow syrup and was taken to the next step without further purification (818 mg, 100%). 1H NMR (500 MHz, CDCL3) δ(ppm): 4.91 (2H, bs), 6.94 (1H, dt, J=8.4, 0.8 Hz), 7.02 (1H, ddd, J=7.2, 5.0, 0.8 Hz), 7.16 (2H, d, J=8.6 Hz), 7.66 (2H, d, J=8.6 Hz), 7.71 (1H, ddd, J=8.2, 7.2, 2.0 Hz), 8.21 (1H, ddd, J=5.0, 2.0, 0.8 Hz). 13C NMR (125 MHz, CDCL3) δ(ppm): 112.1 (CH), 119.1 (CH), 121.4 (CH), 127.6 (CH), 129.0, 139.8 (CH), 147.9 (CH), 152.4, 155.8, 163.4. MS (FAB+): 230 (MH+). HRMS for C12H11N3O2 (MH+): calculated: 230.0930; found 230.0934.

후처리

  1. temperaturethe mixture was refluxed for 16 hours
  2. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-05c5a7f94b12490181955175429d7166
출처 데이터셋
uspto-grants-2015_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09045442B2

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