O-Xylene → 6-(4-Methoxyphenyl)-3-phenyl-[1,2,4]triazolo[3,4-a]phthalazine

HRID 1990782ノート

反応式

HRID 1990782 の反応式
[C:1]([NH:9][NH2:10])(=O)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.Cl.C(N(CC)CC)C.C1(C)C(C)=CC=CC=1.Cl[C:28]1[C:37]2[C:32](=[CH:33][CH:34]=[CH:35][CH:36]=2)[C:31]([C:38]2[CH:43]=[CH:42][C:41]([O:44][CH3:45])=[CH:40][CH:39]=2)=[N:30][N:29]=1>O>[CH3:45][O:44][C:41]1[CH:42]=[CH:43][C:38]([C:31]2[C:32]3[C:37](=[CH:36][CH:35]=[CH:34][CH:33]=3)[C:28]3=[N:10][N:9]=[C:1]([C:2]4[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=4)[N:29]3[N:30]=2)=[CH:39][CH:40]=1

参加物

6

反応物 4

HCID 7237O-XyleneHCID 11130Triethylamine hydrochlorideHCID 11955BenzoylhydrazineHCID 27723901-Chloro-4-(4-methoxyphenyl)phthalazine

生成物 1

HCID 19806306-(4-Methoxyphenyl)-3-phenyl-[1,2,4]triazolo[3,4-a]phthalazine収率 99.3%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

163 mg (1.2 mmol) of benzohydrazide and 165 mg (1.2 mmol) of triethylamine hydrochloride were added to a xylene solution (5 ml) of 271 mg (1.0 mmol) of the obtained 1-chloro-4-(4-methoxyphenyl)-phthalazine, and then stirred under reflux for 2 hours. Water was added to the reaction liquid, extracted with ethyl acetate, and the organic layer was washed with saturated saline water. This was dried with anhydrous sodium sulfate, and concentrated under reduced pressure to obtain 350 mg of a crude product of 6-(4-methoxyphenyl)-3-phenyl-[1,2,4]triazolo[3,4-a]phthalazine.

後処理

  1. temperatureunder reflux for 2 hours
  2. extractionextracted with ethyl acetate
  3. washthe organic layer was washed with saturated saline water
  4. dry with materialThis was dried with anhydrous sodium sulfate
  5. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-99c7ea2fee2d44129dd0051ae79afdc9
出典データセット
uspto-grants-2010_01
特許番号
US07645756B2

反応ノート

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