[CH3:1]C(C)([O-])C.[K+].CN(C)[CH2:9][CH2:10][S:11]([NH:14][C:15]1[CH:20]=[CH:19][C:18]([N+:21]([O-:23])=[O:22])=[CH:17][CH:16]=1)(=[O:13])=[O:12].CI.O>CS(C)=O>[N+:21]([C:18]1[CH:19]=[CH:20][C:15]([N:14]([CH3:1])[S:11]([CH:10]=[CH2:9])(=[O:13])=[O:12])=[CH:16][CH:17]=1)([O-:23])=[O:22]
0.49 g (4.4 mmol) of potassium tert.butoxide are added at ambient temperature to a solution of 1.1 g (4 mmol) of 4-(2-dimethylamino-ethylsulphonylamino)-nitrobenzene (Example 379a) in 20 ml of DMSO. After 1.5 hours stirring 0.85 g (6 mmol) of methyl iodide are added. The mixture is stirred for 18 hours, then the reaction solution is poured into water and extracted with ethyl acetate. The combined organic phases are dried over magnesium sulphate and the solvent is eliminated in vacuo. 0.9 g of ethenesulphonic acid-N-(4-nitrophenyl)-N-methyl-amide are obtained as a crude product. 0.75 g of this crude product are dissolved in ethanol and combined with an excess of dimethylamine. After 18 hours stirring the mixture is evaporated to dryness.
Wird geladen…
