Acetic Acid → HCID 86741486, compound

Participants

Reaction Steps

A mixture of 1.2 parts of 3-[2-[4-(4-fluorobenzoyl)-1-piperidinyl]ethyl]-6-nitro-2,4(1H,3H)-quinazolinedione, 0.5 parts of a solution of thiophene in methanol 4% and 100 parts of acetic acid was hydrogenated at normal pressure and at room temperature with 1 part of platinum-on-charcoal catalyst 5%. After the calculated amount of hydrogen was taken up, the catalyst was filtered off and 10 parts of acetic acid anhydride were added to the filtrate. The whole was stirred and refluxed for 3 hours. After evaporation, water was added to the residue and the whole was treated with ammonia. The precipitated product was filtered off and converted into the (Z)-2-butenedioate salt in ethanol. From the latter the salt was crystallized at -5° C. The product was filtered off and dried, yielding 0.4 parts (32%) of N-[3-[2-[4-(4-fluorobenzoyl)-1-piperidinyl]ethyl]-1,2,3,4-tetrahydro-2,4-dioxo-6-quinazolinyl]-acetamide (Z)-2-butenedioate(1:1).monohydrate; mp. 170.7° C. (15).

Provenance & Evidence