反应详情

A mixture of 120.5 g of 4-hydroxy-4'-nitrostilbene, 69 g of anhydrous potassium carbonate, 143 g of 2,2-dimethyl-4-(4-methyl phenyl sulphonyloxymethyl)-1,3-dioxolane, prepared in accordance with the specification of K. Freudenberg and H. Hess in Liebigs Annalen der Chemie Vol. 448 (1926), p. 121, and 1 l of dimethyl formamide (DMF) was boiled for 30 minutes with refluxing. After cooling the reaction mixture was poured, with vigorous stirring, into 5 l of water. The precipitated crystals were filtered off and after-washed with 5 1 of water. The crude product after drying was crystallized from 4 l of acetone. Obtained were 135 g of 4-((2,2-dimethyl)-1,3-dioxa-4-cyclopentyl)methyl)-4'nitrostilbene in the form of yellow acicular crystals having a melting point of 146°-147° C.

1. customprepared in accordance with the specification of K
2. temperaturewith refluxing
3. temperatureAfter cooling the reaction mixture
4. filtrationThe precipitated crystals were filtered off
5. washafter-washed with 5 1 of water
6. dry with materialThe crude product after drying
7. customwas crystallized from 4 l of acetone
8. customObtained