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llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
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Water → HCID 90065715、化合物

HRID 522268
ノート
印刷プレビュー

反応式

HRID 522268 の反応式
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
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

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

生成物 1

HCID 90065715HCID 90065715、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-cf53543d7ee146ec9193e49a36a89379
出典データセット
uspto-grants-2016_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09328118B2

反応ノート

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