反应详情

温度

120 °C

To a solution of 3-bromo-5-(diethoxymethyl)-2-nitrothiophene (Int. 66) (1 g, 3.22 mmol) in MeOH (10 ml) copper(II) oxide (0.051 g, 0.645 mmol), KI (10.7 mg, 0.064 mmol) and sodium methanolate (0.662 g, 12.25 mmol) were added, and the mixture was heated under MW irradiation at 120° C. for 2 hours. The reaction mixture was filtered through a celite pad, the filtrate was concentrated under vacuum and then partitioned between 0.5N HCl and EtOAc. The organic phase was dried over sodium sulfate, filtered and evaporated to give 5-(diethoxymethyl)-3-methoxy-2-nitrothiophene (Int. 67) (680 mg, 2.60 mmol, MS/ESI+261.0 [MH]+). This crude was used without any additional purification.

1. filtrationThe reaction mixture was filtered through a celite pad
2. concentrationthe filtrate was concentrated under vacuum
3. custompartitioned between 0.5N HCl and EtOAc
4. dry with materialThe organic phase was dried over sodium sulfate
5. filtrationfiltered
6. customevaporated