HRID1518590

反应详情

EQUATION

反应方程式

HRID 1518590 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a mixture of 2-methoxy-4-methylbenzoic acid (20 g, 120.4 mmol), EDC (23.1 g, 120.4 mmol) and HOBt (16.3 g, 120.4 mmol) in dichloromethane (1 L) was added NH3 (7N in MeOH, 52 mL, 3 eq) dropwise. The reaction mixture was stirred at room temperature overnight then washed successively with HCl (1N), saturated aq.NaHCO3, water and brine, dried over MgSO4, filtered and evaporated. The residue was recrystallized from ethyl acetate/hexane to give 16.5 gr of 2-methoxy-4-methylbenzamide (83% yield).

WORKUP

后处理

  1. washthen washed successively with HCl (1N)
  2. dry with materialNaHCO3, water and brine, dried over MgSO4
  3. filtrationfiltered
  4. customevaporated
  5. customThe residue was recrystallized from ethyl acetate/hexane