Hydrochloric Acid → 5-Pyrimidinol, 1,4,5,6-tetrahydro-5-phenyl-, monohydrochloride

Participants

Reaction Conditions

Reaction Steps

A mixture consisting of 5.56 g (0.0335 mol) of 1,3-diamino-2-phenylpropan-2-ol dihydrochloride (m.p. (inst.)=242° C.) and 2.479 g (0.0335 mol; 2.7 ml) of ethyl formate is heated at 100° C. for 3 h. It is then heated at 100° C. under reduced pressure (vacuum obtained by means of a water-jet pump) for 1 h. The reaction medium is cooled, taken up with CH3OH, acidified with ethanol containing HCl and evaporated to dryness, and the evaporation residue is triturated with ether, acetone and chloroform. The precipitate formed is collected by filtration and then recrystallized from an ethanol/diethyl ether mixture (1:1 v/v) to give 6 g (yield: 84%) of CRL 41 382. M.p. (inst.)=206° C.

Provenance & Evidence