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Water → HCID 69732453, 화합물

HRID 896595
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HRID 896595 반응식
[C:1]1([C:11]([N:13]2[C:17](=[O:18])[C:16]([C:25]3[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=3)([C:19]3[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=3)[NH:15][C:14]2=[O:31])=[O:12])[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=[CH:3][CH:2]=1.[H-].[Na+].[CH3:34]I.O>CN(C=O)C>[CH3:34][N:15]1[C:16]([C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)([C:25]2[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=2)[C:17](=[O:18])[N:13]([C:11]([C:1]2[C:10]3[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=3)[CH:4]=[CH:3][CH:2]=2)=[O:12])[C:14]1=[O:31]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 962WaterHCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 12112009HCID 12112009, 화합물

생성물 1

HCID 69732453HCID 69732453, 화합물수율 61.9%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

3-Naphthylcarbonyl-5,5-diphenylimidazolidine-2,4-dione (100 mg) was dissolved in DMF (4 mL), and sodium hydride (60%, in oil) (10 mg) was added at 0° C. under ice-cooling. After stirred for 30 minutes, methyl iodide (37 mg) was added at 0° C., and the mixture was stirred at room temperature overnight. Water (100 mL) was added to the reaction solution, and separated out white precipitates were filtered. Further recrystallization using hexane:ethyl acetate=1:1 afforded 64 mg of white crystals.

후처리

  1. temperaturecooling
  2. stirringthe mixture was stirred at room temperature overnight
  3. customseparated out white
  4. customprecipitates
  5. filtrationwere filtered
  6. customFurther recrystallization

출처 및 근거

ORD 기록
ord-3904369abf714350a4b30296254a0bce
출처 데이터셋
uspto-grants-2005_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06919365B2

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