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

HRID 619685

反応式

HRID 619685 の反応式
[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

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-665e51ad9b7543fe8ead1b6b9ca316c0
出典データセット
uspto-grants-1999_09
特許番号
US05959113

関連ノート

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