[NH2:1][C:2]1[S:3][CH:4]=[C:5]([CH3:12])[C:6]=1[C:7]([O:9][CH2:10][CH3:11])=[O:8].[CH2:13]([N:15]([CH2:18]C)CC)C.C(Cl)(Cl)=[O:21].CN>O1CCCC1>[CH3:12][C:5]1[C:6]([C:7]([O:9][CH2:10][CH3:11])=[O:8])=[C:2]([NH:1][C:13]([NH:15][CH3:18])=[O:21])[S:3][CH:4]=1To a stirred ice-cooled solution of ethyl 2-amino-4-methyl-thiophene-3-carboxylate (1,85 g, 10 mmole) and triethyl amine (1,4 ml, 10 mmol) in dry tetrahydrofuran (50 ml) was added dropwise a phosgene solution (11 mmol, in toluene). The mixture was thereafter heated to reflux for 30 min, then cooled to room temperature and exposed to a gaseous stream of methylamine for 5 min. After additional stirring for 15 min, the mixture was filtered and the filtrate was evaporated to give the title compound as white crystals.
Wird geladen…
