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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 59574309、化合物

HRID 2092038
ノート
印刷プレビュー

反応式

HRID 2092038 の反応式
[O:1]=[C:2]1[C:7]([CH2:8][N:9]2[C:17](=[O:18])[C:16]3[C:11](=[CH:12][CH:13]=[CH:14][CH:15]=3)[C:10]2=[O:19])=[CH:6][CH:5]=[N:4][NH:3]1.[C:20](=O)([O-])[O-].[K+].[K+].CI.O>CN(C)C=O>[CH3:20][N:3]1[C:2](=[O:1])[C:7]([CH2:8][N:9]2[C:10](=[O:19])[C:11]3[C:16](=[CH:15][CH:14]=[CH:13][CH:12]=3)[C:17]2=[O:18])=[CH:6][CH:5]=[N:4]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 595748042-[(3-Oxo-2,3-dihydropyridazin-4-yl)methyl]isoindoline-1,3-dione

生成物 1

HCID 59574309HCID 59574309、化合物収率 86.5%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

2-[(3-Oxo-2,3-dihydropyridazin-4-yl)methyl]isoindoline-1,3-dione (255 mg, 1.00 mmol) in dimethylformamide (3 mL) was heated with potassium carbonate (145 mg, 1.05 mmol) and methyl iodide (426 mg, 3.00 mmol) at 70° C. for 2 hours. After completion of the reaction, the solvent was removed by vacuum distillation, and the resulting residue was stirred with 4 M hydrogen chloride/1,4-dioxane (10 mL) at room temperature for 2 hours. After completion of the reaction, the reaction solution was mixed with water and extracted with ethyl acetate, and the extract was dried over anhydrous magnesium sulfate and evaporated under reduced pressure. The resulting residue was purified by silica gel column chromatography (ethyl acetate) to give the desired product (233 mg, 86% yield).

後処理

  1. customAfter completion of the reaction
  2. customthe solvent was removed by vacuum distillation
  3. customAfter completion of the reaction
  4. extractionextracted with ethyl acetate
  5. dry with materialthe extract was dried over anhydrous magnesium sulfate
  6. customevaporated under reduced pressure
  7. customThe resulting residue was purified by silica gel column chromatography (ethyl acetate)

出典と根拠

ORDレコード
ord-48127662b74b4fc8b5511337d6e04bbc
出典データセット
uspto-grants-2013_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08440666B2

反応ノート

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