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Hydrochloric Acid → 8-Ethoxycarbonylamino-5-hydroxy-3,4-dihydrocarbostyril

HRID 26030
ノート
印刷プレビュー

反応式

HRID 26030 の反応式
Cl.[NH2:2][C:3]1[CH:4]=[CH:5][C:6]([OH:14])=[C:7]2[C:12]=1[NH:11][C:10](=[O:13])[CH2:9][CH2:8]2.[C:15](Cl)(=[O:19])[O:16][CH2:17][CH3:18].Cl>[OH-].[Na+]>[CH2:17]([O:16][C:15]([NH:2][C:3]1[CH:4]=[CH:5][C:6]([OH:14])=[C:7]2[C:12]=1[NH:11][C:10](=[O:13])[CH2:9][CH2:8]2)=[O:19])[CH3:18]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 10928Ethyl chloroformateHCID 213263748-Amino-5-hydroxy-3,4-dihydrocarbostyril hydrochloride

生成物 1

HCID 213263318-Ethoxycarbonylamino-5-hydroxy-3,4-dihydrocarbostyril収率 63.8%

試薬・触媒・溶媒 1

HCID 14798Sodium Hydroxide溶媒

実験手順

10.7 g of 8-amino-5-hydroxy-3,4-dihydrocarbostyril hydrochloride was dissolved in 200 ml of a 10% aqueous sodium hydroxide solution, 5.4 g of ethyl chlorocarbonate was added to the solution while stirring at room temperature followed by stirring for one hour at 30° C. After completion of the reaction, the reaction mixture was rendered acidic with hydrochloric acid under ice-cooling, the precipitated crystals were recovered by filtration, washed with water and dried. Recrystallization of the dried crystals from ethanol yielded 7.95 g of 8-ethoxycarbonylamino-5-hydroxy-3,4-dihydrocarbostyril as colorless needle crystals having a melting point of 283.8°-284.6° C.

後処理

  1. additionwas added to the solution
  2. stirringby stirring for one hour at 30° C
  3. customAfter completion of the reaction
  4. temperaturecooling
  5. filtrationthe precipitated crystals were recovered by filtration
  6. washwashed with water
  7. customdried
  8. customRecrystallization of the dried crystals from ethanol

出典と根拠

ORDレコード
ord-2f095236fcff477d8053be58951e9ded
出典データセット
uspto-grants-1979_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04147869

反応ノート

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