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

HRID 1990782노트

반응식

HRID 1990782 반응식
[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

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-99c7ea2fee2d44129dd0051ae79afdc9
출처 데이터셋
uspto-grants-2010_01
특허 번호
US07645756B2

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