Thionyl Chloride → 6,11-Dihydro-11-oxo-dibenzo[b,e]thiepine-2-acetic acid
반응식
S(Cl)(Cl)=O.C([O:7][C:8](=[O:27])[CH2:9][C:10]1[CH:15]=[CH:14][C:13]([S:16][CH2:17][C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][C:19]=2[C:24]([OH:26])=O)=[CH:12][CH:11]=1)C>>[O:26]=[C:24]1[C:19]2[CH:20]=[CH:21][CH:22]=[CH:23][C:18]=2[CH2:17][S:16][C:13]2[CH:14]=[CH:15][C:10]([CH2:9][C:8]([OH:7])=[O:27])=[CH:11][C:12]1=2참가 물질
3
실험 절차
66 cc of thionyl chloride are added at room temperature to 13.2 g of 4-(2-carboxy-benzyl-thio)phenyl-acetic acid ethyl ester and the mixture is stirred for 90 minutes until gas evolution stops. The mixture is completely concentrated by evaporation at reduced pressure and the resulting light yellow oil is dissolved in ether, whereby 4-(2-chloro-carbonyl-benzyl-thio)phenyl-acetic acid ethyl ester precipitates in the form of light yellow crystals. M.P. 78°-79°.
후처리
- concentrationThe mixture is completely concentrated by evaporation at reduced pressure
- dissolutionthe resulting light yellow oil is dissolved in ether
- customwhereby 4-(2-chloro-carbonyl-benzyl-thio)phenyl-acetic acid ethyl ester precipitates in the form of light yellow crystals