HRID2251959
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
Dissolve [2-(2-chloro-benzoyl)-phenyl]-carbamic acid tert-butyl ester (850 mg, 2.6 mmol) in a saturated HCl in AcOH solution (10 mL, ˜3N in HCl), stir at room temperature for 3 hours. Concentrate, add CHCl3 and concentrate (3×) to remove remaining AcOH. Dissolve the residue in 20% i-PrOH/CHCl3, wash with saturated NaHCO3 solution (2×) and brine. Dry the combined organic layers over MgSO4 and concentrate to afford the title compound (495 mg, 83%): MS(IS) 232 (M+1).
WORKUP
后处理
- concentrationConcentrate
- additionadd CHCl3
- concentrationconcentrate (3×)
- customto remove
- dissolutionDissolve the residue in 20% i-PrOH/CHCl3
- washwash with saturated NaHCO3 solution (2×) and brine
- dry with materialDry the combined organic layers over MgSO4
- concentrationconcentrate