Ethylene Glycol → 2-(2,6-Dimethyl-3-nitrophenyl)-1,3-dioxolane

HRID 619685

반응식

HRID 619685 반응식
[CH3:1][C:2]1[C:9]([N+:10]([O-:12])=[O:11])=[CH:8][CH:7]=[C:6]([CH3:13])[C:3]=1[CH:4]=[O:5].[CH2:14](O)[CH2:15][OH:16].C1(C)C=CC(S(O)(=O)=O)=CC=1.O>C1(C)C=CC=CC=1>[CH3:1][C:2]1[C:9]([N+:10]([O-:12])=[O:11])=[CH:8][CH:7]=[C:6]([CH3:13])[C:3]=1[CH:4]1[O:16][CH2:15][CH2:14][O:5]1

참가 물질

6

반응물 4

HCID 174Ethylene GlycolHCID 962WaterHCID 6101p-Toluenesulfonic acidHCID 218470162,6-Dimethyl-3-nitrobenzaldehyde

생성물 1

HCID 218470332-(2,6-Dimethyl-3-nitrophenyl)-1,3-dioxolane

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

A solution of 2.8 g of 2,6-dimethyl-3-nitrobenzaldehyde in 150 ml of toluene was treated with 5 ml of ethylene glycol and 20 mg of p-toluenesulphonic acid. The mixture was heated to reflux for 18 hours, with the water being separated using a separator. The mixture was left to cool to room temperature and was washed twice with water. After drying over anhydrous magnesium sulphate the solvent was evaporated and the crystalline residue was crystallized from hexane. 3.0 g of 2-(2,6-dimethyl-3-nitrophenyl)-1,3-dioxolane, m.p. 69-71° C., were obtained.

후처리

  1. temperatureThe mixture was heated
  2. customseparated
  3. waitThe mixture was left
  4. washwas washed twice with water
  5. dry with materialAfter drying over anhydrous magnesium sulphate the solvent
  6. customwas evaporated
  7. customthe crystalline residue was crystallized from hexane

출처 및 근거

ORD 기록
ord-665e51ad9b7543fe8ead1b6b9ca316c0
출처 데이터셋
uspto-grants-1999_09
특허 번호
US05959113

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