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Sulfuric Acid → 3-(2-Cyanophenyl)-5-(2-pyridyl)-1-phenyl-1,2-dihydropyridin-2-one sulfate

HRID 2238573
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HRID 2238573 반응식
[S:1](=[O:5])(=[O:4])([OH:3])[OH:2].[C:6]([C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=1[C:14]1[C:15](=[O:32])[N:16]([C:26]2[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=2)[CH:17]=[C:18]([C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][N:21]=2)[CH:19]=1)#[N:7]>O1CCCC1>[S:1]([OH:5])([OH:4])(=[O:3])=[O:2].[C:6]([C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=1[C:14]1[C:15](=[O:32])[N:16]([C:26]2[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=2)[CH:17]=[C:18]([C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][N:21]=2)[CH:19]=1)#[N:7]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 1118Sulfuric AcidHCID 9924495Perampanel

생성물 1

HCID 177513363-(2-Cyanophenyl)-5-(2-pyridyl)-1-phenyl-1,2-dihydropyridin-2-one sulfate수율 343.3%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

A mixture of concentrated sulfuric acid (60 μL, 1.08 mmol) and tetrahydrofuran (5 mL) was added under cooling with ice to a mixture of 3-(2-cyanophenyl)-5-(2-pyridyl)-1-phenyl-1,2-dihydropyridin-2-one (200 mg, 0.138 mmol) and tetrahydrofuran (20 mL), which was then stirred under cooling with ice for one hour. The precipitated solid was collected by filtration, washed with ethyl acetate (small amount), and then dried under reduced pressure to provide 212 mg of the title compound as white crystals.

후처리

  1. additionwas added
  2. temperatureunder cooling with ice for one hour
  3. filtrationThe precipitated solid was collected by filtration
  4. washwashed with ethyl acetate (small amount)
  5. customdried under reduced pressure

출처 및 근거

ORD 기록
ord-8774c3681db94ded8f04eff0bc6d09b3
출처 데이터셋
uspto-grants-2010_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07718807B2

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