반응식
[CH3:1][C:2]1[CH:7]=[C:6]([CH3:8])[CH:5]=[C:4]([CH3:9])[C:3]=1[CH2:10][C:11]([OH:13])=[O:12].[CH3:14]O>Cl>[CH3:9][C:4]1[CH:5]=[C:6]([CH3:8])[CH:7]=[C:2]([CH3:1])[C:3]=1[CH2:10][C:11]([O:13][CH3:14])=[O:12]참가 물질
4
실험 절차
173 g (2,4,6-trimethylphenyl)acetic acid is refluxed in 131 mL of concentrated hydrochloric acid and 1.1 L of methanol for 3 hours with stirring. The solvent is distilled off under reduced pressure and the aqueous phase extracted twice with diethyl ether. The combined organic phases are extracted twice with a saturated aqueous sodium hydrogen carbonate solution and dried with sodium sulfate and the solvent is distilled off under reduced pressure. The residue is fractionally distilled. Yield: 116 g (57%); bp15: 140° C.
후처리
- distillationThe solvent is distilled off under reduced pressure
- extractionthe aqueous phase extracted twice with diethyl ether
- extractionThe combined organic phases are extracted twice with a saturated aqueous sodium hydrogen carbonate solution
- dry with materialdried with sodium sulfate
- distillationthe solvent is distilled off under reduced pressure
- distillationThe residue is fractionally distilled
- custom140° C.
출처 및 근거
- ORD 기록
- ord-56a1a7153101422e84cefdf59ad6caac
- 출처 데이터셋
- uspto-grants-2005_10
- 특허 번호
- US06951888B2
연결된 노트
불러오는 중…