反应详情

温度

0 °C

1.8 g (11.0 mmol) CDT were added to a solution of 3.2 g (10.2 mmol) of ethyl (R)-2-amino-3-(4-amino-3-chloro-5-trifluoromethyl-phenyl)-propionate and 1.8 mL (10.3 mmol) ethyldiisopropylamine in 150 mL THF cooled to 0° C. and the reaction mixture was stirred for 45 min at this temperature and after removal of the ice bath stirred for a further 30 min. Then 2.5 g (10.2 mmol) 3-piperidin-4-yl-1,3,4,5-tetrahydro-1,3-benzodiazepin-2-one suspended in 50 mL THF were added. 40 mL DMF were added to the reaction solution and this was stirred for 2 h at 80° C. It was evaporated down i.vac., combined with 200 mL EtOAc and 200 mL 10% citric acid solution, the organic phase was separated off, extracted with 150 mL NaHCO3 solution and dried over Na2SO4. After elimination of the desiccant and solvent the desired product was obtained.

1. customafter removal of the ice bath
2. stirringstirred for a further 30 min
3. additionwere added
4. stirringthis was stirred for 2 h at 80° C
5. customIt was evaporated down i.vac
6. customthe organic phase was separated off
7. extractionextracted with 150 mL NaHCO3 solution
8. dry with materialdried over Na2SO4