Isopropanol → HCID 21441211, compound

Participants

Reaction Conditions

Reaction Steps

Methylhydrazine (1.0 g, 0.022 mole) is added at 60° C-70° C with stirring to an isopropanol (200 ml) solution of 1,3-dicyclohexyl-2-methyl-1,3-propanedione (5.0 g, 0.02 mole) having a m.p. =36°--37° C and prepared by the procedure of Example 3 above. The reaction is heated at reflux for 4 hours, then cooled, water (300 ml) added and the resulting solid filtered off. The solid is dissolved in anhydrous toluene, methyl hydrazine (1.0 g, 0.022 mole) added and the reaction mixture heated at 90° C for 4 hours. Then additional methyl hydrazine (1.0 g, 0.022 mole) is added and heating continued for 3 hours. The reaction mixture is cooled. The solvent removed on a rotary evaporator and the resulting solid crystallized from hexane/benzene to give 1.7 g (32%) of the desired product, m.p. 120° C to 122° C.

Provenance & Evidence