Triphenylphosphine → HCID 20061205, compound

Participants

Reaction Steps

1.54 g of 2-amino-4-nitrophenol, 2.82 g of 1,3-dimethyl-6-[4-(3-hydroxypropyl)piperazin-1-yl]-2,4(1H,3H)-pyrimidinedione (Compound 139) and 2.88 g of triphenylphosphine were suspended in 20 ml of anhydrous tetrahydrofuran, followed by the addition of 1.92 g of diethyl azodicarboxylate. The thus-prepared mixture was stirred for 1 hour at room temperature and a precipitate was collected by filtration. The precipitate was washed with chloroform-ether to obtain 1.44 g of crytals. The crystals were recrystallized from ethanol-chloroform, thereby obtaining 0.6 g of 1,3-dimethyl-6-{4-[3-(2-amino-4-nitrophenyloxy)propyl]piperazin-1-yl}-2,4(1H,3H)-pyrimidinedione as crystals.

Provenance & Evidence