Water → HCID 67061179、化合物

HRID 598405ノート

反応式

HRID 598405 の反応式
[F:1][C:2]1[CH:7]=[C:6]([I:8])[CH:5]=[CH:4][C:3]=1[NH:9][C:10]1[C:15]([N+:16]([O-:18])=[O:17])=[CH:14][NH:13][C:12](=[O:19])[CH:11]=1.[H-].[Na+].[CH3:22]I.O>CN(C=O)C>[F:1][C:2]1[CH:7]=[C:6]([I:8])[CH:5]=[CH:4][C:3]=1[NH:9][C:10]1[C:15]([N+:16]([O-:18])=[O:17])=[CH:14][N:13]([CH3:22])[C:12](=[O:19])[CH:11]=1

参加物

6

反応物 4

HCID 962WaterHCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 57438270HCID 57438270、化合物

生成物 1

HCID 67061179HCID 67061179、化合物収率 77%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
0 °C

実験手順

4-(2-Fluoro-4-iodophenylamino)-5-nitropyridin-2(1H)-one (1.28 g, 3.41 mmol) was dissolved in dry DMF (20 mL) and cooled to 0° C. under an ice-bath. To the solution was added NaH (60% in oil) (168 mg, 4.2 mmol) portion-wise. The resulted mixture was stirred at 0° C. for 1 hour, followed by the addition of methyl iodide (260 uL, 4.17 mmol) drop-wise through a syringe. The solution was allowed to warm to room temperature and stirred for 16 hours. Water (20 mL) was added slowly and stirring was continued for 30 minutes. The resulted yellow precipitate was filtered, dried under vacuum at 40° C. for 5 hours, and used for the next reaction without further purification. (1.017 g, 77% yield)

後処理

  1. temperatureto warm to room temperature
  2. stirringstirred for 16 hours
  3. stirringstirring
  4. waitwas continued for 30 minutes
  5. filtrationThe resulted yellow precipitate was filtered
  6. customdried under vacuum at 40° C. for 5 hours
  7. customused for the next reaction without further purification

出典と根拠

ORDレコード
ord-96f34065de1f44698d53c8ef9ba892a7
出典データセット
uspto-grants-2011_03
特許番号
US07897624B2

反応ノート

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