Water → 2-methyl-4-(4-isopropylphenyl)-1-(2H)-phthalazinone

HRID 1769141노트

반응식

HRID 1769141 반응식
[CH3:1][NH:2][NH2:3].[CH:4]([C:7]1[CH:23]=[CH:22][C:10]([C:11]([C:13]2[CH:21]=[CH:20][CH:19]=[CH:18][C:14]=2[C:15](O)=[O:16])=O)=[CH:9][CH:8]=1)([CH3:6])[CH3:5].O>C1(C)C=CC=CC=1>[CH3:1][N:2]1[N:3]=[C:11]([C:10]2[CH:9]=[CH:8][C:7]([CH:4]([CH3:5])[CH3:6])=[CH:23][CH:22]=2)[C:13]2[C:14](=[CH:18][CH:19]=[CH:20][CH:21]=2)[C:15]1=[O:16]

참가 물질

5

반응물 3

HCID 962WaterHCID 6061MethylhydrazineHCID 3457982-(4-Isopropylbenzoyl)benzoic acid

생성물 1

HCID 199571122-methyl-4-(4-isopropylphenyl)-1-(2H)-phthalazinone수율 67%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

Methyl hydrazine (8.05 g, 0.175 mol) was added to a mixture of 2-(4-isopropylbenzoyl)benzoic acid (40.2 g, 0.15 mol) in toluene (350 mL) and the mixture was heated to reflux for 3 hours with the removal of water with a Dean Stark trap. The reaction mixture was hot filtered through celite, the filtrate was concentrated to 125 mL and the filtrate was diluted with hexane (100 mL) and cooled. A solid was collected by filtration to afford 27.97 g (67%) of 2-methyl-4-(4-isopropylphenyl)-1-(2H)-phthalazinone, m.p. 107°-107.5° C.

후처리

  1. temperaturethe mixture was heated
  2. filtrationThe reaction mixture was hot filtered through celite
  3. concentrationthe filtrate was concentrated to 125 mL
  4. additionthe filtrate was diluted with hexane (100 mL)
  5. temperaturecooled
  6. filtrationA solid was collected by filtration

출처 및 근거

ORD 기록
ord-4f63687a030b47e3960f4c3475503186
출처 데이터셋
uspto-grants-1995_01
특허 번호
US05380721

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