Ethylene Glycol → 2-(3-Chloropropyl)-2-phenyl-1,3-dioxolane
반응식
[Cl:1][CH2:2][CH2:3][CH2:4][C:5]([C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1)=[O:6].[CH2:13](O)[CH2:14][OH:15]>C1(C)C=CC(S(O)(=O)=O)=CC=1.C1C=CC=CC=1>[Cl:1][CH2:2][CH2:3][CH2:4][C:5]1([C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=2)[O:15][CH2:14][CH2:13][O:6]1참가 물질
5
실험 절차
Add 4-chlorobutyrophenone (50 g, 274 mmol), ethylene glycol (28 g, 452 mmol) and p-toluenesulfonic acid (1.04 g, 5.48 mmol) to benzene (600 mL) and heat at reflux for 16 h under a water trap. Cool the reaction to RT and wash with 1 N NaOH (500 mL) and brine (750 mL). Dry (sodium sulfate) and concentrate to give a solid. Recrystallize the solid from hot hexanes to give the title compound as a white powder (38 g, 61%).
후처리
- temperatureheat
- temperatureat reflux for 16 h under a water trap
- temperatureCool
- customthe reaction to RT
- washwash with 1 N NaOH (500 mL) and brine (750 mL)
- dry with materialDry (sodium sulfate)
- concentrationconcentrate
- customto give a solid
- customRecrystallize the solid from hot hexanes
출처 및 근거
- ORD 기록
- ord-f23fd0818d4a409d927aac3ae6131070
- 출처 데이터셋
- uspto-grants-2011_07
- 특허 번호
- US07981882B2
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