Reacción #556528

Ecuación de reacción

6-(2-chloro-3-methyl-pyridine-4-carbonyl)-4-methyl-3H-benzoxazol-2-one

4-methyl-3H-benzoxazol-2-one

aluminium trichloride

→

6-(2-chloro-5-methyl-pyridine-4-carbonyl)-4-methyl-3H-benzoxazol-2-one

Condiciones de reacción

Tratamiento posterior

1. 1
   Otrothe precipitated grease was separated from the solvent
2. 2
   Otroby decanting
3. 3
   OtroThe residue was triturated with MeOH
4. 4
   OtroThe precipitate formed
5. 5
   Filtraciónfiltered
6. 6
   Lavadowashed with MeOH and diethyl ether
7. 7
   Otrodried i
8. 8
   OtroThe product thus obtained
9. 9
   Otrowas reacted further without further purification

Procedimiento

1.53 g (10.0 mmol) 3-methyl-1-oxy-isonicotinic acid were stirred with 9.32 mL (100 mmol) phosphorus oxychloride and boiled for 4 h. The reaction mixture was evaporated to dryness i. vac. and coevaporated twice with toluene. The crude product thus obtained (which was present in admixture with 2-chloro-3-methyl-isonicotinic acid chloride) was combined with 1.49 g (10.0 mmol) 4-methyl-3H-benzoxazol-2-one and 5.33 g (40.0 mmol) aluminium trichloride and heated to 125° C. for 1.5 h with stirring. Then the mixture was mixed with ice water and the precipitated grease was separated from the solvent by decanting. The residue was triturated with MeOH. The precipitate formed was suction filtered, washed with MeOH and diethyl ether and dried i. vac. The product thus obtained, which was present in admixture with 6-(2-chloro-3-methyl-pyridine-4-carbonyl)-4-methyl-3H-benzoxazol-2-one, was reacted further without further purification.

Fuente