反応式
[CH2:1]([O:3][C:4](=[O:30])[C:5](=P(C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1)[CH2:6][C:7]([F:10])([F:9])[F:8])[CH3:2].O.[F:32][C:33]([F:37])([F:36])[CH:34]=O>C1COCC1>[CH2:1]([O:3][C:4](=[O:30])[C:5]([CH2:6][C:7]([F:8])([F:9])[F:10])=[CH:34][C:33]([F:37])([F:36])[F:32])[CH3:2]参加物
4
反応条件
- 温度
- 100 °C
実験手順
To a solution of 4,4,4-trifluoro-2-(triphenyl-λ5-phosphanylidene)-butyric acid ethyl ester (2.0 g, 4.65 mmol) in THF (5 mL) was added 1 mL of trifluoroacetaldehyde hydrate (tech.). The mixture was sealed in a pressure tube and heated at 100° C. for 3.5 h. After cooling to 23° C., the reaction mixture was eluted through a pad of silica gel (100 g) and Na2SO4 with Et2O (100 mL) to remove the by-products triphenylphosphine oxide and water. The eluent was distilled to remove Et2O and to afford the product as a colorless liquid (1.0 g, 86%).
後処理
- customThe mixture was sealed in a pressure tube
- temperatureAfter cooling to 23° C.
- washthe reaction mixture was eluted through a pad of silica gel (100 g) and Na2SO4 with Et2O (100 mL)
- customto remove the by-products triphenylphosphine oxide and water
- distillationThe eluent was distilled
- customto remove Et2O
出典と根拠
- ORDレコード
- ord-e258429c95244f978a203d3c7c534238
- 出典データセット
- uspto-grants-2009_06
- 特許番号
- US07547725B2
関連ノート
読み込み中…