Thiophene → HCID 13851198, compound

Participants

Reaction Conditions

Reaction Steps

A mixture of 4.85 parts of 7-amino-3-[2-[4-(4-fluorobenzoyl)-1-piperidinyl]ethyl]-2,4(1H,3H)-quinazolinedione dihydrochloride, 4 parts of potassium acetate, 300 parts of 2-methoxyethanol, 1 part of a solution of thiophene in methanol 4% and 4 parts of poly(oxymethylene) was hydrogenated at normal pressure and at 60° C. with 2 parts of palladium-on-charcoal catalyst 5%. After the calculated amount of hydrogen was taken up (about 8 days), the reaction mixture was diluted with 270 parts of N,N-dimethylacetamide and heated to 100° C. The catalyst was filtered off over diatomaceous earth. The filtrate was stirred and cooled and 100 parts of water were added. The precipitated product was filtered off, washed with water and stirred in 2-propanone. The product was filtered off and dried, yielding 2.3 parts (52%) of 7-(dimethylamino)-3-[2-[4-(4-fluorobenzoyl)-1-piperidinyl]ethyl]-2,4(1H ,3H)-quinazolinedione; mp. 300° C. (31).

Provenance & Evidence