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

HRID 54995ノート

反応式

HRID 54995 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-d46f1f2c94fc44ec92b392a644c3a265
出典データセット
uspto-grants-1997_04
特許番号
US05624922

反応ノート

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