反应详情

A mixture of N-(trans-4-trifluoromethyl-cyclohex-1-yl)-2-(difluoromethoxy)-5-amino-4-nitro-benzoic acid amide (70 mg, 0.176 mmol), Pd/C (15 mg) and 10 mL THF is stirred under a H2-atmosphere (3 bar) for 2 h. The crude mixture is filtered into a flask charged with N-(2,4-dichloro-3-isothiocyanato-benzyl)-2,2-dimethyl-propionamide (59 mg, 0.185 mmol) and the filter cake is washed with 40 mL THF. The mixture is stirred for 4 h at rt and overnight at 60° C. Then the reaction mixture is concentrated to −10 mL and stirred for additional 8 h at 60° C. Then it is concentrated i. vac., diluted with MeCN (2.0 mL) and DIC (29 μl, 0.186 mmol) is added and it is stirred for 4 d. Then the mixture is concentrated, diluted with DMF and THF and purified via HPLC.

1. filtrationThe crude mixture is filtered into a flask
2. washthe filter cake is washed with 40 mL THF
3. stirringThe mixture is stirred for 4 h at rt and overnight at 60° C
4. concentrationThen the reaction mixture is concentrated to −10 mL
5. stirringstirred for additional 8 h at 60° C
6. concentrationThen it is concentrated i
7. additionis added
8. stirringit is stirred for 4 d
9. concentrationThen the mixture is concentrated
10. additiondiluted with DMF and THF
11. custompurified via HPLC