HRID469317

反应详情

EQUATION

反应方程式

HRID 469317 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

3.00 g (14.3 mmol) 2,6-dichloropyridine-4-carboxylic acid chloride, 1.80 g (11.0 mmol) 4-methyl-3H-benzoxazol-2-one and 9.47 g (71.0 mmol) aluminium trichloride were combined and heated for 2 h to 125° C. with stirring. Then the mixture was decomposed with ice water and EtOAc and the phases were separated. The aqueous phase was extracted several times with EtOAc. The organic phases were combined, dried on sodium sulphate, filtered and the filtrate was evaporated down i. vac. The residue was triturated with diethyl ether, the precipitate was suction filtered and dried i. vac.

WORKUP

后处理

  1. temperatureheated for 2 h to 125° C.
  2. customthe phases were separated
  3. extractionThe aqueous phase was extracted several times with EtOAc
  4. customdried on sodium sulphate
  5. filtrationfiltered
  6. customthe filtrate was evaporated down i
  7. customThe residue was triturated with diethyl ether
  8. filtrationfiltered
  9. customdried i