Carbon Tetrachloride → HCID 20554358, compound

Participants

Reaction Conditions

Reaction Steps

12.7 g (0.03 mol) of 5-ethoxycarbonyl-4-(2-isopropylaminoanilino)pyrimidine in 42.2 ml of a 0.1 N. aqueous sodium hydroxide solution are heated for 1 hour under reflux. The solvent is removed on a rotary evaporator and the crystalline residue is dried in vacuo at 60° C. 28.9 g (0.11 mol) of triphenylphosphine and 16.9 g (0.11 mol) of carbon tetrachloride are added to the dry product, dissolved in 150 ml of absolute dioxan, and the mixture is stirred for 5 hours at 80° C. The solvent is removed on a rotary evaporator, and the oily residue which remains is chromatographed on neutral silica gel using 99:1 methylene chloride/methanol as the eluant; yield: 6.3 g, with m.p. 204° to 206° C. (from isopropanol).

Provenance & Evidence