반응 #46793

반응 방정식

Methyl-2-amino-3-nitro-benzoate

→

methyl-2,3-diamino-benzoate

용매

MeOH

반응 조건

후처리

1. 1
   기타The solution was evacuated
2. 2
   세척rinsed with argon several times
3. 3
   workup.ADDITION300 mg palladium on charcoal (10%) were added
4. 4
   기타again the mixture was evacuated
5. 5
   세척rinsed with argon a several times
6. 6
   여과The reaction mixture was filtered over “Celite”
7. 7
   세척the filter residue was washed with 150 mL methanol
8. 8
   농축The filtrate was concentrated under reduced pressure

실험 절차

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.

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