Phosphorus oxychloride → Methyl 4-chloro-6-oxo-1-phenyl-1,6-dihydropyridazine-3-carboxylate

HRID 421878

반응식

HRID 421878 반응식
[CH3:1][O:2][C:3]([C:5]1[C:10](O)=[CH:9][C:8](=[O:12])[N:7]([C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)[N:6]=1)=[O:4].P(Cl)(Cl)([Cl:21])=O>>[CH3:1][O:2][C:3]([C:5]1[C:10]([Cl:21])=[CH:9][C:8](=[O:12])[N:7]([C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)[N:6]=1)=[O:4]

참가 물질

3

반응물 2

HCID 24813Phosphorus oxychlorideHCID 54686161Methyl 1,6-dihydro-4-hydroxy-6-oxo-1-phenyl-3-pyridazinecarboxylate

생성물 1

HCID 2784479Methyl 4-chloro-6-oxo-1-phenyl-1,6-dihydropyridazine-3-carboxylate수율 84%

반응 조건

온도
85 °C

실험 절차

A mixture of 4-hydroxy-6-oxo-1-phenyl-1,6-dihydropyridazine-3-carboxylic acid methyl ester (3.83 g, 15.6 mmol) and phosphorous oxychloride (50 mL) was heated to 85° C. After 20 hours, the reaction mixture was concentrated under reduced pressure. The resulting residue was quenched with water. The precipitate was filtered and dissolved in EtOAc, dried (MgSO4) and concentrated under reduced pressure to yield 3.44 g (84%) of desired product.

후처리

  1. concentrationthe reaction mixture was concentrated under reduced pressure
  2. customThe resulting residue was quenched with water
  3. filtrationThe precipitate was filtered
  4. dissolutiondissolved in EtOAc
  5. dry with materialdried (MgSO4)
  6. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-0d539a506ef44539957b92ef876d0d1a
출처 데이터셋
uspto-grants-2012_01
특허 번호
US08101611B2

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