反应详情

Prepared from INT-60 and INT-18. To a stirring solution of tert-butyl 2-((4-bromobenzyl)amino)acetate INT-60 (2.7 g, 8.99 mmol), 4-(2-(4-methoxy-2-(trifluoromethyl)phenyl)acetamido)benzoic acid INT-18 (3.18 g, 8.99 mmol) and TEA (2.507 mL, 17.99 mmol) in DMF was added PyBOP (4.91 g, 9.44 mmol) at room temperature. After 2 h the reaction mixture was diluted with EA (200 mL) and washed with 1 M HCl (100 mL), NaHCO3 (200 mL) and brine (200 mL). The organics were dried over MgSO4, pre-absorbed onto silica gel and purified by chromatography (EA/hexanes) to afford 5.2 g (91%) of tert-butyl 2-(N-(4-bromobenzyl)-4-(2-(4-methoxy-2-(trifluoromethyl)phenyl)acetamido)benzamido)acetate INT-81 as a white foamy solid. LCMS-ESI (m/z) calculated for C30H30BrF3N2O5: 635; found 579/581 [M-tBu+H]+, tR=2.83 min (Method 10).

1. customPrepared from INT-60 and INT-18
2. washwashed with 1 M HCl (100 mL), NaHCO3 (200 mL) and brine (200 mL)
3. dry with materialThe organics were dried over MgSO4
4. custompre-absorbed onto silica gel
5. custompurified by chromatography (EA/hexanes)