HRID469315

反应详情

EQUATION

反应方程式

HRID 469315 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
130 °C

PROCEDURE

实验过程

1.93 g (10.0 mmol) 6-chloropyrimidine-4-carboxylic acid chloride, 1.80 g (10.9 mmol) 4-methyl-3H-benzothiazol-2-one and 7.33 g (55.0 mmol) aluminium trichloride were combined and heated to 130° C. for 3 h with stirring. The mixture was combined with ice water and EtOAc, the flakes formed were suction filtered and the phases were separated. The aqueous phase was extracted 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 DIPE, the precipitate was suction filtered and dried.

WORKUP

后处理

  1. customthe flakes formed
  2. filtrationwere suction filtered
  3. customthe phases were separated
  4. extractionThe aqueous phase was extracted with EtOAc
  5. customdried on sodium sulphate
  6. filtrationfiltered
  7. customthe filtrate was evaporated down i
  8. customThe residue was triturated with DIPE
  9. filtrationfiltered
  10. customdried