BenzaMide, 2-[(2,5-dichloro-4-pyriMidinyl)aMino]- synthesis

Yield:1042434-76-3 83%

Reaction Conditions:

with N-ethyl-N,N-diisopropylamine in isopropyl alcohol; for 18 h;Heating / reflux;

Steps:

1

Intermediate 1; 2-[(2,5-Dichloro-4-pyrimidinyl)amino]benzamide A round-bottomed flask was charged with 2,4,5-trichloropyrimidine (7 g, 38 mmol), ortho-anthranilamide (6.2 g, 45.8 mmol), diisopropyl-ethylamine (8 mL, 45.8 mmol) and 100 mL isopropanol. The flask was fitted with a reflux condenser and the reaction was heated to reflux and stirred for 18 h. A white solid appeared in the reaction mixture. The reaction was cooled to room temperature, of the volume was removed under vacuum and the solid was filtered off and washed with isopropanol. After drying, the white solid (9 g, 32 mmol, 83% yield) was identified as 2-[(2,5-dichloro-4-pyrimidinyl)amino]benzamide. MS: M(C₁₁H₈Cl₂N₄O)=283.12, (M+H)^-=284 and 286.

References:

US2008/182852,2008,A1 Location in patent:Page/Page column 5