HRID18515

反应详情

EQUATION

反应方程式

HRID 18515 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. customThe solution was evacuated
  2. washrinsed with argon several times
  3. addition300 mg palladium on charcoal (10%) were added
  4. customagain the mixture was evacuated
  5. washrinsed with argon a several times
  6. filtrationThe reaction mixture was filtered over “Celite”
  7. washthe filter residue was washed with 150 mL methanol
  8. concentrationThe filtrate was concentrated under reduced pressure