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Water → HCID 90065715, 화합물

HRID 522268
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HRID 522268 반응식
C(=O)([O-])[O-].[K+].[K+].[CH3:7]I.[Cl:9][C:10]1[N:18]=[C:17]2[C:13]([NH:14][C:15]([CH3:19])=[N:16]2)=[C:12]([Cl:20])[N:11]=1.O>C1COCC1>[Cl:9][C:10]1[N:18]=[C:17]2[C:13]([N:14]=[C:15]([CH3:19])[N:16]2[CH3:7])=[C:12]([Cl:20])[N:11]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 962WaterHCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 121341052,6-Dichloro-8-methyl-9H-purine

생성물 1

HCID 90065715HCID 90065715, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

Potassium carbonate (442 mg) and methyl iodide (0.17 mL) were added to a solution of 2,6-dichloro-8-methyl-7H-purine (500 mg) in THF (5 mL) under ice-cooling, and the mixture was stirred at room temperature for 5 hours. After the reaction mixture was ice-cooled, water was added thereto, extraction thereof was performed using EtOAc, and the extract was washed with water and saturated brine. The organic layer was dried over MgSO4 and filtered, and the filtrate was concentrated under reduced pressure. The residue was purified by silica gel column chromatography (Hex:EtOAc=9:1 to 8:2), whereby 2,6-dichloro-8,9-dimethyl-9H-purine (310 mg) was obtained as a white solid.

후처리

  1. temperaturecooling
  2. temperaturecooled
  3. extractionextraction
  4. washthe extract was washed with water and saturated brine
  5. dry with materialThe organic layer was dried over MgSO4
  6. filtrationfiltered
  7. concentrationthe filtrate was concentrated under reduced pressure
  8. customThe residue was purified by silica gel column chromatography (Hex:EtOAc=9:1 to 8:2)

출처 및 근거

ORD 기록
ord-cf53543d7ee146ec9193e49a36a89379
출처 데이터셋
uspto-grants-2016_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09328118B2

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