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

HRID 1291219노트

반응식

HRID 1291219 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 19096565Water ethanol용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-bd9b7dbfe91846e7a43003a5310b5e7e
출처 데이터셋
uspto-grants-1998_05
특허 번호
US05753664

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