Hydrochloric Acid → HCID 67689502、化合物
反応式
[C:1]([O:6][CH:7]1[CH2:12][CH2:11][CH2:10][CH2:9][CH2:8]1)(=[O:5])[C@H:2]([CH3:4])[OH:3].C(N(CC)CC)C.C(Cl)Cl.[C:23](Cl)(=[O:26])[CH:24]=[CH2:25].Cl>>[C:23]([O:3][C@@H:2]([CH3:4])[C:1]([O:6][CH:7]1[CH2:12][CH2:11][CH2:10][CH2:9][CH2:8]1)=[O:5])(=[O:26])[CH:24]=[CH2:25]参加物
反応条件
- 温度
- -20 °C
実験手順
To a mixture of 10.1 g (58.5 mmol) of cyclohexyl (s)-(-)-lactate, 8.1 g (80.4 mmol) of triethylamine and ml of methylene chloride, 5.7 ml (70.2 mmol) of acryloyl chloride was added dropwise at a temperature of -20° C., and the mixture was stirred at -20° C. for 5.5 hours. On ice cooling, 1N hydrochloric acid was added to the reaction mixture to separate an organic layer, and an aqueous layer was extracted with methylene chloride. Organic layers were combined and washed with successive, saturated sodium bicarbonate solution, water, and saturated sodium chloride solution. The solution was dried over anhydrous magnesium sulfate and filtered, the solvent was distilled off, and 13.5 g of crude (S)-cyclohexyl 2-propenoyloxypropionate was obtained.
後処理
- additionwas added dropwise at a temperature of -20° C.
- customto separate an organic layer
- extractionan aqueous layer was extracted with methylene chloride
- washwashed with successive, saturated sodium bicarbonate solution, water, and saturated sodium chloride solution
- dry with materialThe solution was dried over anhydrous magnesium sulfate
- filtrationfiltered
- distillationthe solvent was distilled off
出典と根拠
- ORDレコード
- ord-78e5e1a0462341f9aa32412978b311ed
- 出典データセット
- uspto-grants-1993_11
- 特許番号
- US05266728
反応ノート
読み込み中…