Ethylene Glycol → 2-(3-Methylthiophen-2-yl)-1,3-dioxolane
반응식
[CH3:1][C:2]1[CH:6]=[CH:5][S:4][C:3]=1[CH:7]=[O:8].[CH2:9](O)[CH2:10][OH:11].C1(C)C=CC(S(O)(=O)=O)=CC=1>C1(C)C=CC=CC=1>[CH3:1][C:2]1[CH:6]=[CH:5][S:4][C:3]=1[CH:7]1[O:11][CH2:10][CH2:9][O:8]1참가 물질
5
실험 절차
A mixture of 3-methylthiophene carboxaldehyde (6.8 g), ethylene glycol (10 ml) and p-toluenesulfonic acid (0.30 g) in toluene (125 ml) was heated at reflux for 18 hours. The reaction mixture was cooled; extracted with 2M aqueous sodium carbonate and then dried with brine and over magnesium sulfate. Analysis of the crude product indicated that the reaction was incomplete so the crude material was re-subjected to the ketalisation conditions as outlined above. The crude material isolated after reprocessing was distilled under reduced pressure (1 mmHg) to give the title compound as a yellow oil.
후처리
- temperaturewas heated
- temperatureat reflux for 18 hours
- temperatureThe reaction mixture was cooled
- extractionextracted with 2M aqueous sodium carbonate
- dry with materialdried with brine and over magnesium sulfate
- customThe crude material isolated
- distillationafter reprocessing was distilled under reduced pressure (1 mmHg)
출처 및 근거
- ORD 기록
- ord-74b822405f8e419aaae0449610e9ed3b
- 출처 데이터셋
- uspto-grants-2006_08
- 특허 번호
- US07091237B2
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