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Ethyl Acetate → HCID 67110403, 화합물

HRID 409310
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HRID 409310 반응식
[N:1]1([C:7]2[S:8][C:9]3[CH:15]=[C:14]([OH:16])[CH:13]=[CH:12][C:10]=3[N:11]=2)[CH2:6][CH2:5][O:4][CH2:3][CH2:2]1.[CH2:17]([O:19][C:20](=[O:22])[CH3:21])[CH3:18].[C:23](=[O:26])([O-])[O-].[K+].[K+].[CH3:29][C:30]([N:32](C)C)=[O:31]>>[CH2:17]([O:19][C:20](=[O:22])[CH2:21][N:32]1[C:30](=[O:31])[C:29]2[C:12](=[CH:10][CH:9]=[C:15]([O:16][C:14]3[CH:13]=[CH:12][C:10]4[N:11]=[C:7]([N:1]5[CH2:2][CH2:3][O:4][CH2:5][CH2:6]5)[S:8][C:9]=4[CH:15]=3)[CH:14]=2)[C:23]1=[O:26])[CH3:18]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 4

HCID 8857Ethyl AcetateHCID 11430Potassium CarbonateHCID 31374DimethylacetamideHCID 6625430HCID 6625430, 화합물

생성물 1

HCID 67110403HCID 67110403, 화합물

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온도
105 °C

실험 절차

A mixture of 2-morpholin-4-yl-benzothiazol-6-ol (238 mg, 1.01 mmol), 5-nitro-1,3-dioxo-1,3-dihydro-isoindol-2-yl)-acetic acid ethyl ester (294 mg, 1.06 mmol), potassium carbonate (167 mg, 1.21 mmol) and dimethylacetamide (6 mL) was stirred at 105° C. for twenty-two hours before it was cooled to room temperature and partitioned between chloroform and water. The organic layer was dried over anhydrous sodium sulfate, concentrated in vacuo and the residue was purified by flash column chromatography on silica gel with a gradient of ethyl acetate and dichloromethane to give the title compound as a yellow solid (259 mg): MS: (+) m/z 468.21 (M+1).

후처리

  1. temperaturewas cooled to room temperature
  2. custompartitioned between chloroform and water
  3. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  4. concentrationconcentrated in vacuo
  5. customthe residue was purified by flash column chromatography on silica gel with a gradient of ethyl acetate and dichloromethane

출처 및 근거

ORD 기록
ord-b62990e1bd8b4452a77a6ccc2ef4c925
출처 데이터셋
uspto-grants-2014_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08759373B2

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