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Sodium Acetate → HCID 15052068, 화합물

HRID 329567
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HRID 329567 반응식
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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 517045Sodium AcetateHCID 15052019HCID 15052019, 화합물

생성물 1

HCID 15052068HCID 15052068, 화합물수율 29.2%

시약·촉매·용매 1

HCID 7918Acetic Anhydride용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-e9eec82169e74651a9ae4c44ff9f2d6e
출처 데이터셋
uspto-grants-1990_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04892578

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