反应详情

温度

45 °C

A reaction mixture of 100 g (0.65 mol) of 2,5-dihydroxyacetophenone in 1 l of acetonitrile, 130 ml (1.55 mol) of pyrrolidine and 290 ml (3.95 mol) of acetone was heated at 45° C. for 8 h. The sol. were then removed i. vac. and the residue was dissolved in 1 l of EA. The organic phase was washed twice with dilute hydrochloric acid, stirred with activated carbon and dried over magnesium sulfate and substantially concentrated. The residue was stirred with petroleum ether and the precipitate was filtered off with suction giving 102 g of 2,2-dimethyl-6-hydroxychroman-4-one, m.p. 161° C.

1. customThe sol. were then removed i
2. dissolutionand the residue was dissolved in 1 l of EA
3. washThe organic phase was washed twice with dilute hydrochloric acid
4. dry with materialdried over magnesium sulfate
5. concentrationsubstantially concentrated
6. stirringThe residue was stirred with petroleum ether
7. filtrationthe precipitate was filtered off with suction