1,3-Dichloro-2-isocyanatobenzene → HCID 57710307, compound

Participants

Reaction Conditions

Reaction Steps

A mixture of 1-[4-(6-methylamino-pyrimidin-4-ylamino)-phenyl]-ethanone (3.77 g, 15.56 mmol), 2,6-dichlorophenyl isocyanate (3.22 g, 17.12 mmol) in dry dioxane (30 mL) is shaken for 16 h at 80° C. After evaporation of the solvent in vacuo, the residue is distributed between ethyl acetate and half-saturated K2CO3 solution. The precipitate is filtered off and washed with H2O and ethyl acetate. The solid residue is suspended in methanol, heated to reflux for several h and the hot yellow suspension filtered. This procedure is repeated once. The residue obtained after the second filtration is washed with CH3OH and dried in vacuo to afford the title compound.

Provenance & Evidence