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

HRID 1291219ノート

反応式

HRID 1291219 の反応式
[C:1]([N:5]1[C:10](=[O:11])[C:9]([Cl:12])=[C:8](Cl)[CH:7]=[N:6]1)([CH3:4])([CH3:3])[CH3:2].[CH3:14][NH:15][CH3:16]>C(O)C.O>[C:1]([N:5]1[C:10](=[O:11])[C:9]([Cl:12])=[C:8]([N:15]([CH3:16])[CH3:14])[CH:7]=[N:6]1)([CH3:4])([CH3:3])[CH3:2]

参加物

4

反応物 2

HCID 674DimethylamineHCID 27822252-Tert-butyl-4,5-dichloro-2,3-dihydropyridazin-3-one

生成物 1

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

試薬・触媒・溶媒 1

HCID 19096565Water ethanol溶媒

実験手順

In ethanol-water (2:1) (45 ml)was dissolved 2-t-butyl-4,5-dichloro-3(2H)-pyridazinone (4.4 g) followed by addition of 50% dimethylamine (7.2 g), and the mixture was stirred at room temperature for 15 hours. After removal of ethanol, the residue was extracted with diethyl ether and the organic layer was washed with saturated aqueous NaCl solution, dried over anhydrous magnesium sulfate, and concentrated to dryness. This residue was washed with n-hexane and dried. White powder, 4.4 g. 1H-NMR (CDCl3) δ: 1.63(9H,s), 3.10(6H,s), 7.57(1H,s).

後処理

  1. customAfter removal of ethanol
  2. extractionthe residue was extracted with diethyl ether
  3. washthe organic layer was washed with saturated aqueous NaCl solution
  4. dry with materialdried over anhydrous magnesium sulfate
  5. concentrationconcentrated to dryness
  6. washThis residue was washed with n-hexane
  7. customdried

出典と根拠

ORDレコード
ord-bd9b7dbfe91846e7a43003a5310b5e7e
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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