Methyl iodide → HCID 58259902、化合物

HRID 1020210ノート

反応式

HRID 1020210 の反応式
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8][C:9]2[C:14]([N+:15]([O-:17])=[O:16])=[CH:13][NH:12][C:11](=[O:18])[CH:10]=2)=[C:4]([F:19])[CH:3]=1.[H-].[Na+].[CH3:22]I>CN(C=O)C>[F:19][C:4]1[CH:3]=[C:2]([Br:1])[CH:7]=[CH:6][C:5]=1[NH:8][C:9]1[C:14]([N+:15]([O-:17])=[O:16])=[CH:13][N:12]([CH3:22])[C:11](=[O:18])[CH:10]=1

参加物

5

反応物 3

HCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 574382734-(4-bromo-2-fluorophenylamino)-5-nitropyridin-2(1H)-one

生成物 1

HCID 58259902HCID 58259902、化合物収率 87%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To the yellow solution of 4-(4-bromo-2-fluorophenylamino)-5-nitropyridin-2(1H)-one (1.235 g, 3.78 mmol) dissolved in dry DMF (15 mL) at −5−>0° C., was added NaH (182 mg, 4.55 mmol) (60% in oil). The color of solution turned into dark brown in 20 min at 0° C. The stirring was continued at r.t. for 40 minutes, followed by the addition of MeI (283 uL, 4.54 mmol) through a syringe at 5° C. The resulted solution was stirred at r.t. for 36 hours. The desired compound started to precipitate out of solution after 20 min of MeI addition. Water was added, and the precipitate was vacuum filtered, washed with water, and dried at 40° C. under a high vacuum for 2.5 hours. The product was used for the next reaction without further purification. (1.12 gram, 87% yield).

後処理

  1. customdark brown in 20 min
  2. customat 0° C

出典と根拠

ORDレコード
ord-f76f3676a1f04b85bf85b593859b642c
出典データセット
uspto-grants-2014_05
特許番号
US08716318B2

反応ノート

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