反应详情

Selenium oxide (4.953 g) is heated to dissolve in 100 ml aqueous dioxane (95:5 dioxane: H2O). The 3-fluoro-4-methoxyacetophenone (5.00 g) is added to the mixture. The resulting mixture is refluxed overnight then coiled. The precipitated selenium metal is filtered. The filtrate is concentrated in vacuo to give a brown thick gum. It is recrystallized from -~200 ml hot H2O, filtered hot and allowed to stand at RT overnight. The precipitated pale pink flake are filtered, washed with H2O and let air dried to give 1-methoxy-2-fluoro-4-glyoxyloylbenzene, which is used directly in the next step.

1. temperatureThe resulting mixture is refluxed overnight
2. filtrationThe precipitated selenium metal is filtered
3. concentrationThe filtrate is concentrated in vacuo
4. customto give a brown thick gum
5. customIt is recrystallized from -~200 ml hot H2O
6. filtrationfiltered hot
7. filtrationThe precipitated pale pink flake are filtered
8. washwashed with H2O
9. customdried