HRID18515
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
3.0 g (15.3 mmol) Methyl-2-amino-3-nitro-benzoate were dissolved in 200 mL abs. MeOH. The solution was evacuated and rinsed with argon several times. 300 mg palladium on charcoal (10%) were added and again the mixture was evacuated and rinsed with argon a several times. Finally argon was exchanged by hydrogen (balloon filled with hydrogen) and the mixture was stirred for 4 h at room temperature. The reaction mixture was filtered over “Celite” and the filter residue was washed with 150 mL methanol. The filtrate was concentrated under reduced pressure to give pure methyl-2,3-diamino-benzoate as a brown oil. Yield: 2.53 g MS (ES+): m/e=167.
WORKUP
后处理
- customThe solution was evacuated
- washrinsed with argon several times
- addition300 mg palladium on charcoal (10%) were added
- customagain the mixture was evacuated
- washrinsed with argon a several times
- filtrationThe reaction mixture was filtered over “Celite”
- washthe filter residue was washed with 150 mL methanol
- concentrationThe filtrate was concentrated under reduced pressure