Azane;hydrate → 6-Isopropylpyridazin-3-amine

HRID 1946450노트

반응식

HRID 1946450 반응식
Cl[C:2]1[N:3]=[N:4][C:5]([CH:8]([CH3:10])[CH3:9])=[CH:6][CH:7]=1.O.[NH3:12]>O>[NH2:12][C:2]1[N:3]=[N:4][C:5]([CH:8]([CH3:10])[CH3:9])=[CH:6][CH:7]=1

참가 물질

4

반응물 2

HCID 12896473Azane;hydrateHCID 178045553-Chloro-6-(propan-2-yl)pyridazine

생성물 1

HCID 230281096-Isopropylpyridazin-3-amine

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
165 °C

실험 절차

3-Chloro-6-isopropylpyridazine (1.60 g, 10.2 mmol) and 28% ammonia water (15.0 ml) were introduced into a sealed tube reactor and stirred under pressure and heating at 140° C. for 24 hours and at 165° C. for 25 hours. The reaction solution was left and cooled, poured into water (30.0 ml), adjusted to pH 9, and extracted 3 times with ethyl acetate. The extracts were combined, dried over anhydrous sodium sulfate, and concentrated under reduced pressure to give crude crystals. The crystals, while being washed with diisopropyl ether-hexane, were filtered to give the title compound as pale brown crystals. The yield was 0.41 g (29.3%).

후처리

  1. waitThe reaction solution was left
  2. temperaturecooled
  3. extractionextracted 3 times with ethyl acetate
  4. dry with materialdried over anhydrous sodium sulfate
  5. concentrationconcentrated under reduced pressure
  6. customto give crude crystals
  7. washThe crystals, while being washed with diisopropyl ether-hexane
  8. filtrationwere filtered

출처 및 근거

ORD 기록
ord-76327389dcab4f66b5dd52832d895c8c
출처 데이터셋
uspto-grants-2013_03
특허 번호
US08399381B2

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