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

HRID 1005411노트

반응식

HRID 1005411 반응식
[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]

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-8c790e49cbca485e954af44ba1ed1613
출처 데이터셋
uspto-grants-2000_04
특허 번호
US06054470

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