Ethylene Glycol → 2-(3-Chloro-4-nitrophenyl)-2-methyl-1,3-dioxolane

HRID 1087194ノート

反応式

HRID 1087194 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([C:11](=[O:13])[CH3:12])[CH:5]=[CH:6][C:7]=1[N+:8]([O-:10])=[O:9].[CH2:14](O)[CH2:15][OH:16].O.C1(C)C=CC(S(O)(=O)=O)=CC=1.O>C1(C)C=CC=CC=1>[Cl:1][C:2]1[CH:3]=[C:4]([C:11]2([CH3:12])[O:16][CH2:15][CH2:14][O:13]2)[CH:5]=[CH:6][C:7]=1[N+:8]([O-:10])=[O:9]

参加物

6

反応物 4

HCID 174Ethylene GlycolHCID 962WaterHCID 521998p-Toluenesulfonic acid monohydrateHCID 104427551-(3-Chloro-4-nitrophenyl)ethanone

生成物 1

HCID 100374432-(3-Chloro-4-nitrophenyl)-2-methyl-1,3-dioxolane収率 106.5%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

A solution of 3'-chloro-4'-nitroacetophenone (3 g), ethylene glycol (9.3 g), and p-toluenesulfonic acid monohydrate (0.5 g) in toluene (30 ml) was refluxed for 6 hours. Water formed in the reaction was removed by means of Dean Stark apparatus. The reaction mixture was washed with an aqueous solution of sodium bicarbonate, dried over magnesium sulfate, and concentrated to give an oil of 2-(3-chloro-4-nitrophenyl)-2-methyl-1,3-dioxolane (3.9 g).

後処理

  1. customwas removed by means of Dean Stark apparatus
  2. washThe reaction mixture was washed with an aqueous solution of sodium bicarbonate
  3. dry with materialdried over magnesium sulfate
  4. concentrationconcentrated

出典と根拠

ORDレコード
ord-935a3af827f3481e9370e71a95cf18c4
出典データセット
uspto-grants-1991_07
特許番号
US05034417

反応ノート

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