反应详情

温度

80 °C

A solution of compound 9a (45 mg, 0.092 mmol), methyl bromoacetate (0.053 mL, 0.56 mmol), and potassium carbonate (38 mg, 0.27 mmol) in DMF (1 mL) was sealed in a pressure tube and heated at 80° C. overnight and at rt for two days. Additional methyl bromoacetate (0.060 mL) and potassium carbonate (42 mg) was added and the reaction was heated at 100° C. for 5 h. The reaction mixture was filtered and concentrated on a rotary evaporator. The residue was purified by preparative tlc. This compound was dissolved in a mixture of THF (1 mL) containing several drops of MeOH and 10% LiOH (1 mL). The reaction mixture was stirred at rt for 4 h, neutralized, and concentrated on a rotary evaporator. The residue was dissolved in ethyl acetate, washed with water, dried, and concentrated to give compound 22a (31 mg, 62%). ESI-MS m/e 545.4 (M+1).

1. temperaturethe reaction was heated at 100° C. for 5 h
2. filtrationThe reaction mixture was filtered
3. concentrationconcentrated on a rotary evaporator
4. customThe residue was purified by preparative tlc
5. dissolutionThis compound was dissolved in a mixture of THF (1 mL)
6. additioncontaining several drops of MeOH and 10% LiOH (1 mL)
7. concentrationneutralized, and concentrated on a rotary evaporator
8. dissolutionThe residue was dissolved in ethyl acetate
9. washwashed with water
10. customdried
11. concentrationconcentrated