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Hydrochloric Acid → 7-carboxy-1-isopropyl-4-(m-methoxyphenyl)-2(1H)-quinazolinone

HRID 1834763
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HRID 1834763 반응식
[CH:1]([N:4]1[C:13]2[C:8](=[CH:9][CH:10]=[C:11](C)[CH:12]=2)[C:7]([C:15]2[CH:20]=[CH:19][CH:18]=[C:17]([O:21][CH3:22])[CH:16]=2)=[N:6][C:5]1=[O:23])([CH3:3])[CH3:2].[C:24](=[O:27])([O-])[O-:25].[Na+].[Na+].[Mn]([O-])(=O)(=O)=O.[K+].Cl.S([O-])([O-])(=O)=O.[Na+].[Na+]>[O-2].[O-2].[Mn+4].O>[C:24]([C:11]1[CH:12]=[C:13]2[C:8]([C:7]([C:15]3[CH:20]=[CH:19][CH:18]=[C:17]([O:21][CH3:22])[CH:16]=3)=[N:6][C:5](=[O:23])[N:4]2[CH:1]([CH3:3])[CH3:2])=[CH:9][CH:10]=1)([OH:25])=[O:27]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 5

HCID 313Hydrochloric AcidHCID 10340Sodium CarbonateHCID 24436Sodium SulfateHCID 516875Potassium Permanganate2회HCID 46200211-isopropyl-7-methyl-4-(m-methoxyphenyl)-2(1H)-quinazolinone

생성물 1

HCID 203719547-carboxy-1-isopropyl-4-(m-methoxyphenyl)-2(1H)-quinazolinone

시약·촉매·용매 2

HCID 178418406HCID 178418406, 화합물촉매HCID 962Water용매

실험 절차

A mixture of 11.25 g. of 1-isopropyl-7-methyl-4-(m-methoxyphenyl)-2(1H)-quinazolinone, 5.25 g. of sodium carbonate and 750 ml. of water is refluxed with 7.5 g. of potassium permanganate being added every half hour until a total of 52.5 g. of potassium permanganate is added. After refluxing for an additional 45 minutes, the reaction mixture is cooled, acidified on the slow addition of 263 ml. of 6N. hydrochloric acid and then treated with sodium sulfate until the manganese dioxide is eliminated. The resulting mixture is cooled and filtered to recover the precipitate which is washed with water, dried under vacuum (40° C.) and crystallized from hot glacial acidic acid to obtain 7-carboxy-1--isopropyl-4-(m-methoxyphenyl)-2(1H)-quinazolinone.

후처리

  1. additionA mixture of 11.25 g
  2. temperatureAfter refluxing for an additional 45 minutes
  3. temperaturethe reaction mixture is cooled
  4. additionacidified on the slow addition of 263 ml
  5. temperatureThe resulting mixture is cooled
  6. filtrationfiltered
  7. customto recover the precipitate which
  8. washis washed with water
  9. customdried under vacuum (40° C.)
  10. customcrystallized from hot glacial acidic acid

출처 및 근거

ORD 기록
ord-6f76a33996e44893ae40eab844634f71
출처 데이터셋
uspto-grants-1978_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04071516

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