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

HRID 1990781노트

반응식

HRID 1990781 반응식
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

참가 물질

4

반응물 2

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

생성물 1

HCID 27723901-Chloro-4-(4-methoxyphenyl)phthalazine수율 74%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-0e13dff9a00a4448aee64b25cee35169
출처 데이터셋
uspto-grants-2010_01
특허 번호
US07645756B2

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