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Pyridine → HCID 136335776, 화합물

HRID 2105129
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HRID 2105129 반응식
[NH:1]([C:8]1[N:13]=[C:12]([CH:14]=O)[CH:11]=[CH:10][N:9]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.Cl.[NH2:17][OH:18].N1C=CC=CC=1>CCO>[NH:1]([C:8]1[N:13]=[C:12]([CH:14]=[N:17][OH:18])[CH:11]=[CH:10][N:9]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 1049PyridineHCID 443297Hydroxyamine hydrochlorideHCID 578078012-Anilinopyrimidine-4-carbaldehyde

생성물 1

HCID 136335776HCID 136335776, 화합물수율 92.1%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A suspension of 2-anilinopyrimidin-4-carbaldehyde (Method 3; 10 g, 50 mmol) and hydroxylamine hydrochloride (17.4 g, 250 mmol) in EtOH (360 ml) and pyridine (17.4 g, 215 mmol) was stirred and heated at reflux for 1 hour. The reaction mixture was allowed to cool and concentrated to about 150 ml total volume by evaporation. Distilled water (600 ml) was added and the precipitated solid collected by filtration, washed thoroughly with distilled water and dried to give the title compound (9.86 g, 92%) as a white solid. NMR: 6.92 (t, 1H), 7.08 (d, 1H), 7.23 (t, 2H), 7.75 (d, 2H), 7.93 (s, 1H), 8.45 (d, 1H), 9.67 (s, 1H), 12.1 (s, 1H); m/z 215.

후처리

  1. temperatureheated
  2. temperatureat reflux for 1 hour
  3. temperatureto cool
  4. concentrationconcentrated to about 150 ml total volume by evaporation
  5. additionDistilled water (600 ml) was added
  6. filtrationthe precipitated solid collected by filtration
  7. washwashed thoroughly with distilled water
  8. customdried

출처 및 근거

ORD 기록
ord-d292d4ed96034014964be8956fed39a4
출처 데이터셋
uspto-grants-2009_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07579344B2

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