反応式
[S:1]1[CH:5]=[CH:4][CH:3]=[C:2]1[CH2:6][CH2:7][C:8](O)=[O:9]>C1COCC1>[S:1]1[CH:5]=[CH:4][CH:3]=[C:2]1[CH2:6][CH2:7][CH2:8][OH:9]参加物
3
反応条件
- 温度
- 0 °C
実験手順
Borane methylsulfide complex (6.4 mL, 12.8 mmol) was added to a solution of 3-(2-thienyl)propanoic acid (1.0 g, 6.4 mmol) in THF (18 mL) at 0° C. The reaction mixture was stirred at 0° C. for 2 hours and at room temperature for 3 additional hours. After cooling down to 0° C., the reaction was quenched by addition of a saturated solution of potassium carbonate (5 mL). The aqueous layer was separated and extracted with ethyl acetate (2×15 mL) and diethyl ether (2×15 mL). The combined organic phases were dried over sodium sulfate, filtered and concentrated to dryness. The title compound was obtained as a colorless oil (1.0 g, 100%).
後処理
- temperatureAfter cooling down to 0° C.
- customthe reaction was quenched by addition of a saturated solution of potassium carbonate (5 mL)
- customThe aqueous layer was separated
- extractionextracted with ethyl acetate (2×15 mL) and diethyl ether (2×15 mL)
- dry with materialThe combined organic phases were dried over sodium sulfate
- filtrationfiltered
- concentrationconcentrated to dryness
出典と根拠
- ORDレコード
- ord-63cc154a584f4c0dbb69321ff3330cc5
- 出典データセット
- uspto-grants-2014_09
- 特許番号
- US08846711B2
関連ノート
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