Potassium Carbonate → 1363593-70-7

Reaktionsgleichung

C(OC(=O)[N:7]([S:11]([C:14]1[CH:19]=[C:18]([Br:20])[CH:17]=[CH:16][C:15]=1[OH:21])(=[O:13])=[O:12])[CH2:8][CH2:9]Cl)(C)(C)C.C([O-])([O-])=O.[K+].[K+]>C(O)C.CCCCCCC>[Br:20][C:18]1[CH:17]=[CH:16][C:15]2[O:21][CH2:9][CH2:8][NH:7][S:11](=[O:13])(=[O:12])[C:14]=2[CH:19]=1

Komponenten

Versuchsvorschrift

37 g (81 mmol) of the product obtained in Step D above are heated at reflux in the presence of 2.69 g (16 mmol) of KI and 33.6 g (240 mmol) of K2CO3 in 1.2 L of ethanol for about 18 hours. After cooling, the salts are filtered off and rinsed with acetone. After evaporation, the filtrate is taken up in water. The mixture is acidified with 1N HCl solution and then extracted 3 times with CH2Cl2. The organic phase is washed twice with brine, dried over MgSO4 and evaporated. The residue obtained (˜22 g) is then triturated in heptane, and then the mixture is allowed to separate in order to remove the heptane supernatant. The residue is again triturated in a heptane/isopropyl ether mixture to obtain a solid. After filtration, the product is rapidly dried and then ground in a mortar. The solid obtained is dissolved in heptane, stirred for about 1 hour and filtered to yield the expected product.