HRID9089

反应详情

EQUATION

反应方程式

HRID 9089 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. concentrationThe solution was concentrated under reduced pressure
  2. additionthe residue was diluted with EtOAc (700 mL)
  3. washwashed with 5% aq. KHCO3 solution (400 mL, 2×), water, and brine
  4. dry with materialdried (MgSO4)
  5. filtrationfiltered
  6. concentrationconcentrated
  7. washThe residue was washed with ether (200 mL) and acetonitrile (100 mL)