反应详情

A mixture of N-(3-chloro-4-fluorophenyl)-2-(2-fluoroethoxy)-4-methylamino-5-nitro-benzamide (67.9 mg, 0.176 mmol), Pd/C (15 mg) and 10 mL THF is stirred under a H2-atmosphere (3 bar) for 8 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 concentrated to ˜5 mL. The mixture is stirred for 2 h at rt and concentrated i. vac. The mixture is diluted with MeCN (2.0 mL), DIC (29 μl, 0.186 mmol) is added and it is stirred overnight at rt and 2 h at 60° C. The mixture is cooled to rt and the resulting precipitate is filtered off, washed with MeCN, redissolved in dioxane/MeCN and a few drops of HCOOH and lyophilized.

1. filtrationThe crude mixture is filtered into a flask
2. concentrationconcentrated to ˜5 mL
3. stirringThe mixture is stirred for 2 h at rt
4. concentrationconcentrated i
5. additionis added
6. stirringit is stirred overnight at rt and 2 h at 60° C
7. filtrationthe resulting precipitate is filtered off
8. washwashed with MeCN
9. dissolutionredissolved in dioxane/MeCN