Hydrochloric Acid → HCID 59214340、化合物

HRID 552842ノート

反応式

HRID 552842 の反応式
[H-].[Li+].[CH3:3][O:4][C:5]([C:7]1[CH:12]=[CH:11][NH:10][C:9](=[O:13])[CH:8]=1)=[O:6].I[CH2:15][CH:16]([CH3:18])[CH3:17].Cl>CN(C=O)C>[CH3:3][O:4][C:5]([C:7]1[CH:12]=[CH:11][N:10]([CH2:15][CH:16]([CH3:18])[CH3:17])[C:9](=[O:13])[CH:8]=1)=[O:6]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 10556Isobutyl iodideHCID 62714Lithium hydrideHCID 280755Methyl 2-oxo-1,2-dihydropyridine-4-carboxylate

生成物 1

HCID 59214340HCID 59214340、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒3 回

実験手順

LiH (78 mg) was suspended in DMF (5 ml), and a suspension of methyl-2-oxo-1,2-dihydropyridine-4-carboxylate (500 mg) in DMF (5 ml) was added dropwise thereto at room temperature. The suspension was stirred as it was, and a solution of 1-iodo-2-methylpropane (506 μl) in DMF (5 ml) was added dropwise thereto over 10 min, followed by stirring at 50° C. for 15 hours. To the reaction solution was added 1M HCl at 0° C., followed by extraction with EtOAc, and the organic layer was washed with saturated brine, dried over anhydrous MgSO4, and filtered, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel chromatography (n-hexane:EtOAc=90:10 to 50:50) to obtain methyl-1-isobutyl-2-oxo-1,2-dihydropyridine-4-carboxylate (440 mg) as white powders.

後処理

  1. additionwas added dropwise
  2. customat room temperature
  3. stirringby stirring at 50° C. for 15 hours
  4. extractionfollowed by extraction with EtOAc
  5. washthe organic layer was washed with saturated brine
  6. dry with materialdried over anhydrous MgSO4
  7. filtrationfiltered
  8. customthe solvent was evaporated under reduced pressure
  9. customThe residue was purified by silica gel chromatography (n-hexane:EtOAc=90:10 to 50:50)

出典と根拠

ORDレコード
ord-d07f8556e3f54dcfa47f49aeb45f1fed
出典データセット
uspto-grants-2011_05
特許番号
US07951825B2

反応ノート

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