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

HRID 1834763
ノート
印刷プレビュー

反応式

HRID 1834763 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 5

HCID 313Hydrochloric AcidHCID 10340Sodium CarbonateHCID 24436Sodium SulfateHCID 516875Potassium Permanganate2 回HCID 46200211-isopropyl-7-methyl-4-(m-methoxyphenyl)-2(1H)-quinazolinone

生成物 1

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

試薬・触媒・溶媒 2

HCID 178418406HCID 178418406、化合物触媒HCID 962Water溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-6f76a33996e44893ae40eab844634f71
出典データセット
uspto-grants-1978_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04071516

反応ノート

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