Phenol → HCID 18176473, compound

Participants

Reaction Conditions

Reaction Steps

To a solution of 13.10 g (45.5 mmol) 5-benzyl-8-methyl-2,3,4,5-tetrahydro-9(8H)-pyridazino[4,5-b][1,5]thiazepinone in 116 ml of 85% phosphoric acid 5.00 g (53.0 mmol) of phenol are added and the solution is stirred for 3 hours at 150° C. After cooling the solution is poured onto 100 g of ice-water and the pH of the mixture is adjusted to neutral with 138 g of solid sodium carbonate. The precipitate is filtered and the wet filter-cake is boiled with 12×40 ml of isopropanol. The combined isopropanol solutions are evaporated. The residue is triturated with diethyl ether, filtered and washed. In this way 6.50 g (72%) of the title compound are obtained with a melting point of 254-256° C.

Provenance & Evidence