Phosphorus oxychloride → 1-Chloro-4-(4-methoxyphenyl)phthalazine

HRID 1990781ノート

反応式

HRID 1990781 の反応式
P(Cl)(Cl)([Cl:3])=O.[CH3:6][O:7][C:8]1[CH:13]=[CH:12][C:11]([C:14]2[C:23]3[C:18](=[CH:19][CH:20]=[CH:21][CH:22]=3)[C:17](=O)[NH:16][N:15]=2)=[CH:10][CH:9]=1>O>[Cl:3][C:17]1[C:18]2[C:23](=[CH:22][CH:21]=[CH:20][CH:19]=2)[C:14]([C:11]2[CH:12]=[CH:13][C:8]([O:7][CH3:6])=[CH:9][CH:10]=2)=[N:15][N:16]=1

参加物

4

反応物 2

HCID 24813Phosphorus oxychlorideHCID 6891034-(4-Methoxyphenyl)-1-(2H)-phthalazinone

生成物 1

HCID 27723901-Chloro-4-(4-methoxyphenyl)phthalazine収率 74%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

With cooling with ice, 25 ml of phosphorus oxychloride was added to 95.05 g (20 mmol) of the obtained 4-(4-methoxyphenyl)-2H-phthalazin-1-on, and the reaction liquid was stirred under reflux for 6 hours. Water was added to the reaction liquid, extracted with chloroform, and the organic layer was washed with saturated saline water. This was dried with anhydrous sodium sulfate, and concentrated under reduced pressure to obtain 4.00 g (yield: 74%) of 1-chloro-4-(4-methoxyphenyl)-phthalazine as a white solid.

後処理

  1. customthe reaction liquid
  2. temperatureunder reflux for 6 hours
  3. extractionextracted with chloroform
  4. washthe organic layer was washed with saturated saline water
  5. dry with materialThis was dried with anhydrous sodium sulfate
  6. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-0e13dff9a00a4448aee64b25cee35169
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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