HRID469315
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customthe flakes formed
- filtrationwere suction filtered
- customthe phases were separated
- extractionThe aqueous phase was extracted with EtOAc
- customdried on sodium sulphate
- filtrationfiltered
- customthe filtrate was evaporated down i
- customThe residue was triturated with DIPE
- filtrationfiltered
- customdried