反应详情

(1-Chloro-2-methyl-propenyl)-dimethylamine (102 μl) is added to a mixture of 2-(difluoro-methoxy)-5-amino-4-nitro-benzoic acid (175 mg, 0.705 mmol, prepared in analogy to WO2010/034797), 5 mL THF and 10 mL DCM and it is stirred for 5 h. Then trans-4-trifluoromethyl-cyclohexylamine (158 mg, 0.776 mmol) and pyridine (139 μL, 1.77 mmol) are added and it is stirred overnight. The solvent is removed i. vac., half-saturated aq. NaHCO3— solution is added and it is extracted with DCM. The organic layers are dried with Na2SO4, filtered, concentrated and purified via preparative HPLC (Method F).

1. stirringit is stirred overnight
2. customThe solvent is removed i
3. addition, half-saturated aq. NaHCO3— solution is added
4. extractionit is extracted with DCM
5. dry with materialThe organic layers are dried with Na2SO4
6. filtrationfiltered
7. concentrationconcentrated
8. custompurified via preparative HPLC (Method F)