Azane;hydrate → 6-Isopropylpyridazin-3-amine

HRID 1946450ノート

反応式

HRID 1946450 の反応式
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

参加物

4

反応物 2

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

生成物 1

HCID 230281096-Isopropylpyridazin-3-amine

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
165 °C

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-76327389dcab4f66b5dd52832d895c8c
出典データセット
uspto-grants-2013_03
特許番号
US08399381B2

反応ノート

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