Ethanol → 2-(3-Methylphenyl)-2-nitropropane-1,3-diol

HRID 64440노트

반응식

HRID 64440 반응식
[CH3:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([CH2:8][N+:9]([O-:11])=[O:10])[CH:3]=1.[OH-:12].[Na+].[CH2:14]=O.[CH2:16]([OH:18])C>O1CCOCC1>[CH3:1][C:2]1[CH:3]=[C:4]([C:8]([N+:9]([O-:11])=[O:10])([CH2:16][OH:18])[CH2:14][OH:12])[CH:5]=[CH:6][CH:7]=1

참가 물질

6

반응물 4

HCID 702EthanolHCID 712Formaldehyde2회HCID 14798Sodium Hydroxide2회HCID 112865651-Methyl-3-(nitromethyl)benzene

생성물 1

HCID 867134582-(3-Methylphenyl)-2-nitropropane-1,3-diol

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

To a mixed solution of 1.55 g of 1-methyl-3-(nitromethyl)benzene in 15 ml of ethanol and 6 ml of dioxane were added 0.05 ml of a 1 M aqueous sodium hydroxide solution and 1.89 ml of a 37% aqueous formalin solution, followed by stirring for 15 hours. 0.05 ml of a 1 M aqueous sodium hydroxide solution and 0.83 ml of a 37% aqueous formalin solution were added thereto, followed by stirring at 50° C. for 2 hours, and the solvent was evaporated under reduced pressure. To the obtained residue was added ethyl acetate, followed by washing with saturated brine and drying over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure. The obtained residue was purified by silica gel column chromatography to obtain 1.91 g of 2-(3-methylphenyl)-2-nitropropane-1,3-diol.

후처리

  1. stirringby stirring at 50° C. for 2 hours
  2. customthe solvent was evaporated under reduced pressure
  3. additionTo the obtained residue was added ethyl acetate
  4. washby washing with saturated brine
  5. dry with materialdrying over anhydrous magnesium sulfate
  6. customthe solvent was evaporated under reduced pressure
  7. customThe obtained residue was purified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-ff579edcad5a47e4b62f37b3a4aedc9d
출처 데이터셋
uspto-grants-2016_09
특허 번호
US09447090B2

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