HRID9089
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
PROCEDURE
实验过程
A solution of [5-[[(2,4,6-Trimethylphenyl)amino]carbonyl]-4-methyl-2-thiazolyl]carbamic acid, 1,1-dimethylethyl ester (10 g, 26.63 mmol) in trifluoroacetic acid (100 mL) was stirred at rt for 3 h. The solution was concentrated under reduced pressure and the residue was diluted with EtOAc (700 mL), washed with 5% aq. KHCO3 solution (400 mL, 2×), water, and brine; dried (MgSO4), filtered and concentrated. The residue was washed with ether (200 mL) and acetonitrile (100 mL) to obtain the title compound (6.7 g, 91%) as a white solid.
WORKUP
后处理
- concentrationThe solution was concentrated under reduced pressure
- additionthe residue was diluted with EtOAc (700 mL)
- washwashed with 5% aq. KHCO3 solution (400 mL, 2×), water, and brine
- dry with materialdried (MgSO4)
- filtrationfiltered
- concentrationconcentrated
- washThe residue was washed with ether (200 mL) and acetonitrile (100 mL)