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

HRID 1087194노트

반응식

HRID 1087194 반응식
[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]

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-935a3af827f3481e9370e71a95cf18c4
출처 데이터셋
uspto-grants-1991_07
특허 번호
US05034417

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