反应详情

A mixture of N-(trans-4-trifluoromethyl-cyclohexyl)-6-methylamino-5-amino-2-(4-trifluoromethyl-piperidinyl)-nicotinic acid amide (110 mg, 0.24 mmol), N-(4-chloro-3-isothiocyanato-benzyl)-1-trifluoromethyl-cyclopropylcarboxamide (prepared according to WO2010/100249; 80 mg, 0.24 mmol) and MeCN (7.5 mL) is stirred for 5 h. Then DIC (50 μl, 0.32 mmol) is added and it is stirred overnight at rt and for 2 h at 60° C. The crude mixture is diluted with 40% aq. methylamine-solution, filtered, concentrated and purified by prep. HPLC (X-bridge C18 column; water (+0.15% aq. Ammonia)/MeOH 9:1->MeOH).

1. stirringit is stirred overnight at rt and for 2 h at 60° C
2. filtrationfiltered
3. concentrationconcentrated
4. custompurified by prep