N,N-Diethyl-1,3-propanediamine → HCID 136067515, compound

Participants

Reaction Steps

A solution of 10 g (0.031 mol) of ethyl-5-(4-hydroxyphenyl)-4-phenyl-1H-pyrazole-1-acetate of example 6 in 48 mL of diethylaminopropylamine was stirred on a steam bath under nitrogen for 14 hours. The excess amine was removed in vacuo at 80° C., the residue dissolved in ethyl acetate, washed twice with water, once with brine and dried over sodium sulfate. The ethyl acetate was stripped to yield 12 g of a dark oil which was triturated in hot cyclohexane several times. The insoluble residue was combined with a small amount of a mixture of oil and crystals, which had separated from the cyclohexane on cooling, and recrystallized from ethyl acetate to yield 6.6 g of product, mp 110-113.

Provenance & Evidence