3-Chloro-1-butene → 1-(1-Methyl-2-propenyloxy)-5-methyl-2-nitrobenzene

HRID 637625

반응식

HRID 637625 반응식
[H-].[Na+].[CH3:3][C:4]1[CH:5]=[CH:6][C:7]([N+:11]([O-:13])=[O:12])=[C:8]([OH:10])[CH:9]=1.Cl[CH:15]([CH3:18])[CH:16]=[CH2:17].[OH-].[Na+]>CS(C)=O>[CH3:17][CH:16]([O:10][C:8]1[CH:9]=[C:4]([CH3:3])[CH:5]=[CH:6][C:7]=1[N+:11]([O-:13])=[O:12])[CH:15]=[CH2:18]

참가 물질

6

반응물 4

HCID 112423-Chloro-1-buteneHCID 127886-Nitro-m-cresolHCID 14798Sodium HydroxideHCID 24758Sodium hydride

생성물 1

HCID 135602931-(1-Methyl-2-propenyloxy)-5-methyl-2-nitrobenzene

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매

실험 절차

24 g of sodium hydride was added in portions to a stirred mixture of 153 g of 5-methyl-2-nitrophenol and 500 ml of DMSO. Then 135.7 g of 3-chloro-1-butene was added drop-by-drop (over 5 minutes) to the stirred mixture, which then was stirred at reflux (79°-81° C.) for 24 hours. Then the mixture was made basic with 50% aqueous sodium hydroxide, poured over ice water and extracted with methylene chloride. The extract was washed with cold water, dried (MgSO4), filtered and stripped of solvent, to give 1-(1-methyl-2-propenyloxy)-5-methyl-2-nitrobenzene (1A), as a dark-colored syrup.

후처리

  1. temperatureat reflux (79°-81° C.) for 24 hours
  2. extractionextracted with methylene chloride
  3. washThe extract was washed with cold water
  4. dry with materialdried (MgSO4)
  5. filtrationfiltered

출처 및 근거

ORD 기록
ord-89f1cfebad004de6b9345d10f5f19162
출처 데이터셋
uspto-grants-1985_12
특허 번호
US04558040

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