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Sodium Acetate → HCID 19976946, 화합물

HRID 1450666
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HRID 1450666 반응식
[C:1]1([C:7]2[CH:11]=[C:10]([CH:12]([OH:16])[CH2:13][CH2:14][CH3:15])[S:9][N:8]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.C([O-])(=O)C.[Na+].[Cr](Cl)([O-])(=O)=O.[NH+]1C=CC=CC=1>ClCCl>[C:1]1([C:7]2[CH:11]=[C:10]([C:12](=[O:16])[CH2:13][CH2:14][CH3:15])[S:9][N:8]=2)[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 517045Sodium AcetateHCID 19976910HCID 19976910, 화합물HCID 178418287HCID 178418287, 화합물

생성물 1

HCID 19976946HCID 19976946, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To 35 ml of dichloromethane, were added 1.73 g (7.42 mmol) of 3-phenyl-5-(1-hydroxybutyl)isothiazole, 1.1 g (13.4 mmol) of sodium acetate and 2.88 g of "Frolisil" (trade mark). While the resultant mixture was vigorously stirred at room temperature, 2.88 g (13.4 mmol) of pyridinium chlorochromate were added at once. After the reaction mixture was stirred for 2 hours, an insoluble material was filtered off and the solvent was then distilled off. The residue was purified by silica gel chromatography (eluent: 20:1 n-hexane/ethyl acetate), whereby 3-phenyl-5-butyrylisothiazole was obtained as colorless crystals.

후처리

  1. filtrationan insoluble material was filtered off
  2. distillationthe solvent was then distilled off
  3. customThe residue was purified by silica gel chromatography (eluent: 20:1 n-hexane/ethyl acetate)

출처 및 근거

ORD 기록
ord-8a3d08e5af554f9e85a126f17af751e2
출처 데이터셋
uspto-grants-1997_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05602160

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