Sodium Chloride → HCID 9861202、化合物

HRID 1795863ノート

反応式

HRID 1795863 の反応式
[NH:1]1[CH:6]=[C:5]([C:7]2[C:8]([C:16]3[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=3)=[N:9][N:10]3[CH:15]=[CH:14][N:13]=[CH:12][C:11]=23)[CH:4]=[CH:3][C:2]1=[O:22].[H-].[Na+].I[CH3:26].[Na+].[Cl-]>CN(C=O)C>[CH3:26][N:1]1[CH:6]=[C:5]([C:7]2[C:8]([C:16]3[CH:17]=[CH:18][CH:19]=[CH:20][CH:21]=3)=[N:9][N:10]3[CH:15]=[CH:14][N:13]=[CH:12][C:11]=23)[CH:4]=[CH:3][C:2]1=[O:22]

参加物

6

反応物 4

HCID 5234Sodium ChlorideHCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 99219923-(2(1H)-pyridinon-5-yl)-2-phenylpyrazolo[1,5-a] pyrazine

生成物 1

HCID 9861202HCID 9861202、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To a suspension of 3-(2(1H)-pyridinon-5-yl)-2-phenylpyrazolo[1,5-a]pyrazine (120 mg) in DMF (3 mL) was added NaH (60% oil suspension, 25 mg) at room temperature and the mixture was stirred at the same temperature for 10 min. To the mixture was added iodomethane (0.039 mL). After stirring at room temperature for 15 h, the reaction mixture was poured into 10% NaCl solution, extracted with EtOAc, washed with 10% NaCl solution and brine, dried over sodium sulfate, evaporated in vacuo. The residue was purified by silica gel column chromatography (EtOAc to CH2Cl2-MeOH 10:1) to give 3-(1-methyl-2(1H)-pyridinon-5-yl)-2-phenylpyrazolo[1,5-a]pyrazine (114.5 mg) as a solid.

後処理

  1. stirringAfter stirring at room temperature for 15 h
  2. extractionextracted with EtOAc
  3. washwashed with 10% NaCl solution and brine
  4. dry with materialdried over sodium sulfate
  5. customevaporated in vacuo
  6. customThe residue was purified by silica gel column chromatography (EtOAc to CH2Cl2-MeOH 10:1)

出典と根拠

ORDレコード
ord-c7e36082716d4b80a630ad840a98fdc3
出典データセット
uspto-grants-2006_04
特許番号
US07030121B2

反応ノート

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