2-t-butyl-4-chloro-5-dimethylamino-3(2H)-pyridazinone → 2-t-butyl-5-dimethylamino-3(2H)-pyridazinone

HRID 1291220ノート

反応式

HRID 1291220 の反応式
[C:1]([N:5]1[C:10](=[O:11])[C:9](Cl)=[C:8]([N:13]([CH3:15])[CH3:14])[CH:7]=[N:6]1)([CH3:4])([CH3:3])[CH3:2]>CO.[Pd]>[C:1]([N:5]1[C:10](=[O:11])[CH:9]=[C:8]([N:13]([CH3:15])[CH3:14])[CH:7]=[N:6]1)([CH3:4])([CH3:3])[CH3:2]

参加物

4

反応物 1

HCID 189188582-t-butyl-4-chloro-5-dimethylamino-3(2H)-pyridazinone

生成物 1

HCID 189189072-t-butyl-5-dimethylamino-3(2H)-pyridazinone

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 887Methanol溶媒

実験手順

In methanol (40 ml) was dissolved 2-t-butyl-4-chloro-5-dimethylamino-3(2H)-pyridazinone (4.3 g) followed by addition of 10% palladium-on-carbon (water content 50%) (430 mg), and the mixture was stirred under hydrogen at room temperature for 48 hours. The catalyst was then filtered off and the filtrate was concentrated. To the residue was added saturated aqueous NaHCO3 solution and the mixture was extracted with ethyl acetate. The organic layer was washed with saturated aqueous NaCl solution, dried over anhydrous magnesium sulfate, and concentrated to dryness. The residue was washed with n-hexane and dried. White powder, 3.4 g. 1H-NMR (CDC13) 6: 1.63(9H,s), 2.98(6H,s), 5.65(1H,d,J=3.OHz), 7.55(1H,d,J=3.0Hz).

後処理

  1. filtrationThe catalyst was then filtered off
  2. concentrationthe filtrate was concentrated
  3. additionTo the residue was added saturated aqueous NaHCO3 solution
  4. extractionthe mixture was extracted with ethyl acetate
  5. washThe organic layer was washed with saturated aqueous NaCl solution
  6. dry with materialdried over anhydrous magnesium sulfate
  7. concentrationconcentrated to dryness
  8. washThe residue was washed with n-hexane
  9. customdried

出典と根拠

ORDレコード
ord-0bcd0aa615b94f0a8b2260f2032910dc
出典データセット
uspto-grants-1998_05
特許番号
US05753664

反応ノート

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