反应 #1605772

ord-684e4b93eb264e9eb912c3a906b4b0a4

反应方程式

N
NH3
COc1cc(C)ccc1C(=O)O
2-methoxy-4-methylbenzoic acid
ClCCCl
EDC
On1nnc2ccccc21
HOBt
COc1cc(C)ccc1C(N)=O
2-methoxy-4-methylbenzamide
收率 83.0%

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    洗涤then washed successively with HCl (1N)
  2. 2
    干燥NaHCO3, water and brine, dried over MgSO4
  3. 3
    过滤filtered
  4. 4
    其他evaporated
  5. 5
    其他The residue was recrystallized from ethyl acetate/hexane

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).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US09072313B2uspto-grants-2015_07