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Water → HCID 59574309, 화합물

HRID 2092038
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HRID 2092038 반응식
[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
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HCID 962WaterHCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 595748042-[(3-Oxo-2,3-dihydropyridazin-4-yl)methyl]isoindoline-1,3-dione

생성물 1

HCID 59574309HCID 59574309, 화합물수율 86.5%

시약·촉매·용매 1

HCID 6228Dimethylformamide
용매

실험 절차

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).

후처리

  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)

출처 및 근거

ORD 기록
ord-48127662b74b4fc8b5511337d6e04bbc
출처 데이터셋
uspto-grants-2013_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08440666B2

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