Water → 1-Hexyl-5-iodo-4-methyl-3-nitro-2-pyridone

HRID 1387281

反応式

HRID 1387281 の反応式
[I:1][C:2]1[C:3]([CH3:12])=[C:4]([N+:9]([O-:11])=[O:10])[C:5](=[O:8])[NH:6][CH:7]=1.[H-].[Na+].[CH2:15](Br)[CH2:16][CH2:17][CH2:18][CH2:19][CH3:20].O>CN(C=O)C>[CH2:15]([N:6]1[CH:7]=[C:2]([I:1])[C:3]([CH3:12])=[C:4]([N+:9]([O-:11])=[O:10])[C:5]1=[O:8])[CH2:16][CH2:17][CH2:18][CH2:19][CH3:20]

参加物

6

反応物 4

HCID 962WaterHCID 81011-BromohexaneHCID 24758Sodium hydrideHCID 217065145-Iodo-4-methyl-3-nitro-1,2-dihydropyridin-2-one

生成物 1

HCID 217065251-Hexyl-5-iodo-4-methyl-3-nitro-2-pyridone

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A mixture of 5-iodo-4-methyl-3-nitro-2-pyridone (8.0 g, 28.6 mmol) and sodium hydride (1.03 g, 43 mmol) in DMF (150 mL) was stirred at rt for 1 hour. n-Hexyl bromide (8.03 mL, 57.2 mmol) was added, and the mixture was stirred for 24 hours. Water was added, and the mixture was extracted with ethyl acetate. The organic phase was washed, dried, filtered and evaporated. Chromatography of a portion of the residue over silica gel (20% petroleum ether/methylene chloride) gave 1-hexyl-5-iodo-4-methyl-3-nitro-2-pyridone.

後処理

  1. stirringthe mixture was stirred for 24 hours
  2. extractionthe mixture was extracted with ethyl acetate
  3. washThe organic phase was washed
  4. customdried
  5. filtrationfiltered
  6. customevaporated

出典と根拠

ORDレコード
ord-823b466d8ffa47918793c6e56a31c61f
出典データセット
uspto-grants-2001_07
特許番号
US06268365B1

関連ノート

読み込み中…