Water → HCID 19373306, 화합물
반응식
[OH:1][CH2:2][C:3]1([CH2:11][OH:12])[CH2:8][O:7][C:6]([CH3:10])([CH3:9])[O:5][CH2:4]1.[H-].[Na+].[CH2:15](I)[CH3:16].O>CN(C)C=O>[CH3:10][C:6]1([CH3:9])[O:5][CH2:4][C:3]([CH2:11][O:12][CH2:15][CH3:16])([CH2:2][OH:1])[CH2:8][O:7]1참가 물질
6
실험 절차
To a stirred solution of 5,5-di-(hydroxymethyl)-2,2-dimethyl-1,3-dioxane (5.0 g) (Beilstein 19, II, 93) in dry dimethylformamide (50 ml) under nitrogen, at 20°, was added sodium hydride (0.68 g, 80% dispersion in oil). The mixture was stirred at 80° for 2 hours and cooled. Ethyl iodide (4.4 g) in dry dimethylformamide (40 ml) was added and the mixture was heated at 110° for 3 hours. The mixture was cooled and poured into water. The aqueous mixture was extracted with diethyl ether. The ethereal extracts were washed with brine, dried over anhydrous magnesium sulphate and evaporated in vacuo. 2,2-Dimethyl-5-ethoxymethyl-5-hydroxymethyl-1,3-dioxane was obtained as a pale yellow oil (1.2 g) and was used without further purification.
후처리
- temperaturecooled
- temperaturethe mixture was heated at 110° for 3 hours
- temperatureThe mixture was cooled
- extractionThe aqueous mixture was extracted with diethyl ether
- washThe ethereal extracts were washed with brine
- dry with materialdried over anhydrous magnesium sulphate
- customevaporated in vacuo
출처 및 근거
- ORD 기록
- ord-b5a1b2e458c44ca5ac34c337b2034a59
- 출처 데이터셋
- uspto-grants-1992_05
- 특허 번호
- US05116862
반응 노트
불러오는 중…