반응식
[C:1]1([CH:7]([CH3:11])[C:8](O)=[O:9])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.S(Cl)([Cl:14])=O>C(Cl)(Cl)(Cl)Cl>[C:1]1([CH:7]([CH3:11])[C:8]([Cl:14])=[O:9])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1참가 물질
실험 절차
(±)-2-Phenylpropionic acid in the amount of 7.50 g (50 mmol) and 7.14 g (60 mmol) of thionyl chloride were heated for 1 hour under reflux in carbon tetrachloride. The solvent and unaltered thionyl chloride were evaporated under reduced pressure to give (±)-2-phenylpropionic acid chloride as a pale yellow oil. To the oil were added 30 ml of benzene, 7.30 g (52.5 mmol) of p-nitrophenol and 4.75 g (60.0 mmol) of pyridine were added, and the mixture was stirred at room temperature for 2 hours. The reaction mixture was diluted with 10 ml of aqueous 10% hydrochloric acid, extracted with ethyl acetate, followed by solvent evaporation from the organic layer, to obtain 13.9 g of a pale yellow solid. Recrystallization of the solid from ethanol gave 10.4 g (38.4 mmol, yield 77%) of (±)-p-nitrophenyl 2-phenylpropionate as colorless crystals.
후처리
- customThe solvent and unaltered thionyl chloride were evaporated under reduced pressure
출처 및 근거
- ORD 기록
- ord-f37b8ce702804a52a205927d7031fe51
- 출처 데이터셋
- uspto-grants-1987_11
- 특허 번호
- US04709082
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