Triphenylphosphine → 1,3-dimethyl-6-[4-(3-[2-chloro-4-nitrophenyloxy]propyl)piperazin-1-yl]-2,4(1H,3H)-pyrimidinedione

Participants

Reaction Steps

In 70 ml of anhydrous tetrahydrofuran were suspended 2.4 g of 2-chloro-4-nitrophenol, 3.38 g of 1,3-dimethyl-6-[4-(3-hydroxypropyl)piperazin-1-yl]-2,4(1H,3H)-pyrimidinedione (Compound a) and 3.62 g of triphenylphosphine, and 2.4 g of diethyl azodicarboxylate was added to the resultant suspension. Afterward, the resultant mixture was treated in the same manner as in Reference Example 4 to obtain 2.5 g of light yellow crystals. The crystals were recrystallized from ethanol to obtain 2.07 g of crystalline 1,3-dimethyl-6-[4-(3-[2-chloro-4-nitrophenyloxy]propyl)piperazin-1-yl]-2,4(1H,3H)-pyrimidinedione (Compound u).

Provenance & Evidence