Isatoic Anhydride → HCID 14010430, compound

Participants

Reaction Steps

A mixture comprising 1.63 g of 2H-3,1-benzoxazine-2,4(1H)-dione, 1.78 g of ethyl orthoformate and 2.77 g of 4-(2-ethoxyphenyl)-1-(4-aminobutyl)piperazine was heated on a boiling water bath for about 10 minutes and further heated on an oil bath of 120° to 130° C. for about 2 hours. After the completion of the reaction, the reaction mixture was concentrated under a reduced pressure and the residue was columnchromatographed over silica gel column and eluted with an ethyl acetatetriethylamine solvent (30:1) to give 1.5 g of 3-{4-[4-(2-ethoxyphenyl)-1-piperazinyl]butyl}-4(3H)-quinazolone as an oil (yield: 66.7%). ##STR15## 1.50 g of this oily free base was dissolved in a small amount of acetone. The obtained solution was added to a saturated solution of 0.857 g of fumaric acid in acetone to precipitate a crude crystal. The crude crystal was recrystallized from ethanol to give 1.65 g of the corresponding monofumarate having a melting point of 197° to 198° C. as a colorless prisms.

Provenance & Evidence