Methacrolein → 1-(3-Methyl-1,3-butadienyl)-2-nitrobenzene

HRID 374003

반응식

HRID 374003 반응식
O=[CH:2][C:3](=[CH2:5])[CH3:4].[Br-].[N+:7]([C:10]1[CH:35]=[CH:34][CH:33]=[CH:32][C:11]=1[CH2:12][P+](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1)([O-:9])=[O:8].[OH-].[Na+]>C1C=CC=CC=1>[CH3:4][C:3](=[CH2:5])[CH:2]=[CH:12][C:11]1[CH:32]=[CH:33][CH:34]=[CH:35][C:10]=1[N+:7]([O-:9])=[O:8]

참가 물질

5

반응물 3

HCID 6562MethacroleinHCID 14798Sodium HydroxideHCID 10885283(2-Nitrobenzyl)triphenylphosphonium bromide

생성물 1

HCID 537916531-(3-Methyl-1,3-butadienyl)-2-nitrobenzene

시약·촉매·용매 1

HCID 241Benzene용매

실험 절차

5.0 ml of methacrolein was dissolved in 100 ml of benzene. Thereto were added 31.5 g of 2-nitro-benzyltriphenylphosphonium bromide and 100 ml of a 5 N aqueous sodium hydroxide solution. The mixture was stirred at room temperature for 5 hours. The organic layer was separated and washed with an aqueous saturated sodium chloride solution and dried over anhydrous magnesium sulfate. The solvent was removed by distillation under reduced pressure. The residue was purified by column chromatography (eluant: toluene) to obtain 2.7 g of 1-(3-methyl-1,3-butadienyl)-2-nitrobenzene (containing about 2.2 g of o-nitrotoluene) as a light yellow oily material.

후처리

  1. customThe organic layer was separated
  2. washwashed with an aqueous saturated sodium chloride solution
  3. dry with materialdried over anhydrous magnesium sulfate
  4. customThe solvent was removed by distillation under reduced pressure
  5. customThe residue was purified by column chromatography (eluant: toluene)

출처 및 근거

ORD 기록
ord-43144c0ad6ff45aba5b735de56d1b6f5
출처 데이터셋
uspto-grants-1992_11
특허 번호
US05166204

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