Water → 5-Acetyl-5-methyl-1,3-dioxane
반응식
[OH:1][CH2:2][C:3]([CH2:8][OH:9])([CH3:7])[C:4](=[O:6])[CH3:5].[CH2:10]1OCOCO1.C1(C)C=CC(S(O)(=O)=O)=CC=1.O>C1(C)C=CC=CC=1>[C:4]([C:3]1([CH3:7])[CH2:8][O:9][CH2:10][O:1][CH2:2]1)(=[O:6])[CH3:5]참가 물질
6
실험 절차
A solution of 3,3-bis(hydroxymethyl)-2-butanone (66.1parts) and s-trioxane (27 parts) in toluene (250 parts) containing p-toluenesulfonic acid (1.9 parts) is held under reflux while water of reaction is continuously removed (ca. 0.5 hr) by a Dean-Stark trap. The solution is cooled, neutralized by stirring with solid sodium bicarbonate and filtered Toluene is removed in vacuo and the residue distilled at 50-55° C. and 0.6 mm Hg. Proton NMR and combustion analysis are consistent with those values predicted for the desired product. Combustion Analysis for C7H12O3 --Calculated: C, 58.3%; H, 8.4%. Found: C, 57.9%; H, 8.2%.
후처리
- customis continuously removed (ca. 0.5 hr) by a Dean-Stark trap
- temperatureThe solution is cooled
- filtrationfiltered Toluene
- customis removed in vacuo
- distillationthe residue distilled at 50-55° C.
출처 및 근거
- ORD 기록
- ord-7f63e32c62124005acbb76283e70f768
- 출처 데이터셋
- uspto-grants-1992_06
- 특허 번호
- US05118599
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