反应详情

A solution of Boc-Arg(Pbf)-OH (3.33 g, 6.32 mmol), HATU (2.88 g, 7.58 mmol) and DIEA (7.4 mL, 31.6 mmol) in DMF (40 mL) was maintained at room temperature for 20 min, followed by the addition of compound C hydrochloride (1.45 g, 6.95 mmol). Stirring was continued for additional 1 h. The reaction mixture was diluted with EtOAc (500 mL) and extracted with water (3×75 mL) and brine (75 mL). The organic layer was dried over MgSO4 and then evaporated to provide compound AA (4.14 g, 5.77 mmol) as yellowish amorphous solid. LC-MS [M+H] 717.6 (C35H52N6O8S+H, calc: 717.9). Compound AA was used without further purification.

1. extractionextracted with water (3×75 mL) and brine (75 mL)
2. dry with materialThe organic layer was dried over MgSO4
3. customevaporated
4. customto provide compound AA (4.14 g, 5.77 mmol) as yellowish amorphous solid
5. customCompound AA was used without further purification