反应详情

温度

5 °C

To a solution of compound D (8.0 g, 11.1 mmol) in CHCl3 (50 ml) was added DIEA (4.1 mL, 23.3 mmol) at room temperature and stirred for 15 min. The mixture was cooled to ˜5° C., ethyl chloroformate (1.06 mL, 11.1 mmol) was added drop wise. After stirring at room temperature overnight (˜18 h), solvent removed in vacuo. The residue was dissolved in MeOH (˜25 ml) and Et2O (˜500 mL) was added. The precipitated crude product was filtered off, washed with Et2O and dried under vacuo to afford compound E (8.5 g, 11.1 mmol). LC-MS [M+H] 757.6 (C36H48N6O8S2+H, calc: 757.9). Compound E was used without further purification.

1. stirringAfter stirring at room temperature overnight (˜18 h), solvent
2. customremoved in vacuo
3. dissolutionThe residue was dissolved in MeOH (˜25 ml)
4. additionEt2O (˜500 mL) was added
5. customThe precipitated crude product
6. filtrationwas filtered off
7. washwashed with Et2O
8. customdried under vacuo