HCID 642459, compound → HCID 86745602, compound

Participants

Reaction Steps

In a 2-1 three-neck flask equipped with an intensive condenser and a stirrer, 50 g of 3,3,5-trimethylcyclohex-5-ene-1,2,4-trione (from Example 2) were dissolved in 300 ml of concentrated hydrochloric acid at room temperature. The flask was then dipped into a hot oil bath at 100° C. for 15 minutes, in the course of which the reaction mixture turned dark and an orange precipitate formed. This solid precipitate was filtered off with suction while hot and washed with water, ethanol, acetone, ethyl acetate and ether. The resulting product was freed of adhering solvent residues in a desiccator. (It is pure enough in this state for further reactions. If desired, it can be recrystallized from dioxane.)

Provenance & Evidence