반응식
[Na].Cl.Cl[CH2:4][C:5]1[CH:10]=[CH:9][N:8]=[CH:7][CH:6]=1.Cl.[CH:12]([OH:15])([CH3:14])[CH3:13]>>[CH:12]([O:15][CH2:4][C:5]1[CH:10]=[CH:9][N:8]=[CH:7][CH:6]=1)([CH3:14])[CH3:13]참가 물질
5
실험 절차
3.4 g of sodium are dissolved in 120 ml of isopropanol and 11 g (0.067 mol) of 4-chloromethylpyridine-hydrochloride are added. The reaction mixture is refluxed for 10 hours under nitrogen, with stirring, then after cooling it is made weakly acidic with dilute hydrochloric acid and concentrated by evaporation under reduced pressure. The residue is made alkaline with 40% potassium carbonate solution and extracted with ether. After drying with anhydrous sodium sulphate the organic phase is concentrated by evaporation. The crude product is then distilled.
후처리
- temperatureThe reaction mixture is refluxed for 10 hours under nitrogen
- temperatureafter cooling it
- concentrationconcentrated by evaporation under reduced pressure
- extractionextracted with ether
- dry with materialAfter drying with anhydrous sodium sulphate the organic phase
- concentrationis concentrated by evaporation
- distillationThe crude product is then distilled
출처 및 근거
- ORD 기록
- ord-9964c7de6933407d9c2220728e01fc8c
- 출처 데이터셋
- uspto-grants-1995_06
- 특허 번호
- US05422353
연결된 노트
불러오는 중…