반응 #4974
ord-1d5819da44804bb79114f5102ded9ad5
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반응 조건
후처리
- 1기타at 5° C.
- 2기타After the insoluble component was removed
- 3추출the solution was extracted with 100 ml of chloroform
- 4세척washed with saturated brine
- 5건조dried with Glauber's salt
- 6기타After removing Glauber's salt
- 7농축the solution was concentrated under reduced pressure
- 8기타the residue was recrystallized from hot hexane
실험 절차
87 ml of water and 18.2 ml (0.218 mol) of 12N-HCl were added to the solution of 87 ml of chloroform and 8.65 g (0.0121 mol) of the white solid containing 3,5-dihexadecyloxycarbonylbenzenesulfonyl chloride, and then 7.93 g of zinc was added thereto at 5° C. followed by stirring for 4 hours and 30 minutes. After the insoluble component was removed therefrom, the solution was extracted with 100 ml of chloroform, washed with saturated brine, and dried with Glauber's salt. After removing Glauber's salt, the solution was concentrated under reduced pressure, and the residue was recrystallized from hot hexane to obtain a colorless crystal of 3,5-dihexadecyloxycarbonylbenzenesulfonic acid. (Yield: 4.43 g, 48% (based on sodium 3,5-dimethyloxycarbonylbenzenesulfonate), m.p.: 63°-65° C.).