反应详情

温度

0 °C

To a suspension of 6.9 g (40.78 mmol) LiAlH4 in 70 mL diethyl ether under nitrogen was added drop wise a solution of 6.9 g (175 mmol) 2-methyl-5-((E)-2-nitro-vinyl)-thiophene in 150 mL diethyl ether at 20 to 25° C. After complete addition the mixture was heated to reflux for 5 h. The mixture was cooled to 0° C. and 28 mL water and 7 mL 5N NaOH and was added. The white solid was filtered, washed with ethyl acetate and the filtrate was concentrated in vacuo. The residue was distilled at reduced pressure to yield 4.98 g (86%) of the title compound as colourless liquid.

1. additionAfter complete addition the mixture
2. temperaturewas heated
3. temperatureto reflux for 5 h
4. filtrationThe white solid was filtered
5. washwashed with ethyl acetate
6. concentrationthe filtrate was concentrated in vacuo
7. distillationThe residue was distilled at reduced pressure