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Sodium Acetate → HCID 15052068、化合物

HRID 329567
ノート
印刷プレビュー

反応式

HRID 329567 の反応式
C([O-])(=O)C.[Na+].[Cl:6][C:7]1[CH:12]=[C:11]([NH:13][C:14]([C:16]2[C:21]([C:22]([OH:24])=O)=[CH:20][CH:19]=[CH:18][N:17]=2)=[O:15])[CH:10]=[CH:9][C:8]=1[CH2:25][N:26]1[C:30](=[O:31])[C:29]([CH3:33])([CH3:32])[CH2:28][O:27]1>C(OC(=O)C)(=O)C>[Cl:6][C:7]1[CH:12]=[C:11]([N:13]2[C:22](=[O:24])[C:21]3[C:16](=[N:17][CH:18]=[CH:19][CH:20]=3)[C:14]2=[O:15])[CH:10]=[CH:9][C:8]=1[CH2:25][N:26]1[C:30](=[O:31])[C:29]([CH3:33])([CH3:32])[CH2:28][O:27]1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 517045Sodium AcetateHCID 15052019HCID 15052019、化合物

生成物 1

HCID 15052068HCID 15052068、化合物収率 29.2%

試薬・触媒・溶媒 1

HCID 7918Acetic Anhydride溶媒

実験手順

Using a method analogous to that of M. P. Cava et al., supra, a solution of 5.0 grams (0.061 mole) of sodium acetate in 50 mL of acetic anhydride was stirred while heating with a steam bath, and 1.5 grams (0.004 mole) of 2-[[2-chloro-4-[(3-carboxy-2-pyridinyl)carbonylamino]phenyl]methyl]-4,4-dimethyl-3-isoxazolidinone was added in one portion. Upon completion of addition the reaction mixture was heated with the steam bath for an additional 30 minutes. The reaction mixture was poured into 500 mL of ice-water, and the resultant solid was collected by filtration. The solid was recrystallized from acetone-water to yield 0.45 gram of 2-[[2-chloro-4-(pyrrolo[3,4-b]pyridine-5,7-dione-6-yl)phenyl]-methyl]-4,4-dimethyl-3-isoxazolidinone; m.p. 139°-141° C.

後処理

  1. temperaturewhile heating with a steam bath
  2. additionUpon completion of addition the reaction mixture
  3. temperaturewas heated with the steam bath for an additional 30 minutes
  4. filtrationthe resultant solid was collected by filtration
  5. customThe solid was recrystallized from acetone-water

出典と根拠

ORDレコード
ord-e9eec82169e74651a9ae4c44ff9f2d6e
出典データセット
uspto-grants-1990_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04892578

反応ノート

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