反应详情

温度

100 °C

A mixture of Intermediate 7 (80 mg, 0.348 mmol), Intermediate 1 (125 mg, 0.348 mmol) and glyoxylic acid monohydrate (32.0 mg, 0.348 mmol) in DMF (0.3 mL)/acetonitrile (0.900 mL) was heated at 100° C. for 10 min in microwave reactor. A solution of Intermediate 8 (109 mg, 0.348 mmol) in DMF (2 mL) and DIEA (0.182 mL, 1.043 mmol) was added to the reaction mixture, followed by BOP (185 mg, 0.417 mmol) as a solid. The mixture was stirred at rt for 3 h. The reaction mixture was diluted with CH2Cl2 and 0.5 N HCl, extracted with CH2Cl2. The organic layer was washed with brine, dried over Na2SO4, filtered and concentrated. The crude product was purified by prep HPLC. The desired fractions were concentrated, diluted with EtOAc and washed with sat. NaHCO3, dried over Na2SO4, filtered and concentrated to give 5A (100 mg, 0.121 mmol, 34.9% yield). MS (ESI) m/z: 824 [M+1]+.

1. extractionextracted with CH2Cl2
2. washThe organic layer was washed with brine
3. dry with materialdried over Na2SO4
4. filtrationfiltered
5. concentrationconcentrated
6. customThe crude product was purified by prep HPLC
7. concentrationThe desired fractions were concentrated
8. additiondiluted with EtOAc
9. washwashed with sat. NaHCO3
10. dry with materialdried over Na2SO4
11. filtrationfiltered
12. concentrationconcentrated