反应详情

7.0 g of 4-(2-chloro-carbonyl-benzyl-thio)phenylacetic acid ethyl ester are dissolved in 30 cc of nitrobenzene and this solution is added dropwise, at room temperature, to a solution of 3.32 g of aluminium chloride in 50 cc of nitrobenzene. The resulting red solution is then heated in an oil bath of 100° for 3 hours. The reaction solution is subsequently poured on a mixture of ice and 10 N hydrochloric acid, is diluted with ether, and the organic phase is separated, washed with water, dried with sodium sulphate, purified with charcoal and filtered. The solvent is completely removed at reduced pressure and the oily residue is dissolved in ether, the ether phase is washed with a 10% sodium bicarbonate solution and then with water, is dried with sodium sulphate, filtered, and the solvent is removed by distillation at reduced pressure. 6,11-Dihydro-11-oxo-dibenzo[b,e]thiepine-2-acetic acid ethyl ester crystallizes from ether/pentane. M.P. 96°-97°.

1. temperatureThe resulting red solution is then heated in an oil bath of 100° for 3 hours
2. customthe organic phase is separated
3. washwashed with water
4. dry with materialdried with sodium sulphate
5. custompurified with charcoal
6. filtrationfiltered
7. customThe solvent is completely removed at reduced pressure
8. dissolutionthe oily residue is dissolved in ether
9. washthe ether phase is washed with a 10% sodium bicarbonate solution
10. dry with materialwith water, is dried with sodium sulphate
11. filtrationfiltered
12. customthe solvent is removed by distillation at reduced pressure
13. custom6,11-Dihydro-11-oxo-dibenzo[b,e]thiepine-2-acetic acid ethyl ester crystallizes from ether/pentane