反応式
[CH:1]([O:8]CC)([O:5][CH2:6][CH3:7])OCC.[F:11][C:12]([F:19])([F:18])[C:13]([CH3:17])=[CH:14][CH2:15]O.[C:20](O)(=O)CC>C(OCC)C>[CH3:17][C:13]([C:12]([F:19])([F:18])[F:11])([CH:14]=[CH2:15])[CH2:20][C:1]([O:5][CH2:6][CH3:7])=[O:8]参加物
5
反応条件
- 温度
- 200 °C
実験手順
Triethyl orthoformate (6.51 mL, 35.7 mmol) was added to an ambient temperature mixture of 4,4,4-trifluoro-3-methylbut-2-en-1-ol (ca. 500 mg, 3.57 mmol) and propionic acid (13 μL, 0.18 mmol). After heating in a sealed tube at 200° C. for 30 h, the reaction mixture was cooled, diluted with diethyl ether and washed with saturated aqueous sodium bicarbonate. The organic phase was dried (magnesium sulfate) and concentrated in vacuo. Chromatography over silica eluting with 0-20% ethyl acetate/hexane afforded ethyl 3-methyl-3-(trifluoromethyl)pent-4-enoate.
後処理
- temperaturethe reaction mixture was cooled
- washwashed with saturated aqueous sodium bicarbonate
- dry with materialThe organic phase was dried (magnesium sulfate)
- concentrationconcentrated in vacuo
出典と根拠
- ORDレコード
- ord-764fbb9f5e2a4c2cb8ac9fa2da6f71cc
- 出典データセット
- uspto-grants-2012_06
- 特許番号
- US08193228B2
関連ノート
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