반응 #40515

반응 방정식

6-chloro-4-fluoro-8-nitro-9H-β-carboline

ammonium formate

sodium bicarbonate

sodium chloride

→

6-chloro-4-fluoro-9H-β-carbolin-8-ylamine

수율 70.3%

용매

methanol

ethanol

반응 조건

후처리

1. 1
   온도After cooling to RT the mixture
2. 2
   여과was filtered through a short plug of Celite®
3. 3
   세척washing with copious amounts of methanol
4. 4
   농축the filtrate concentrated in vacuo
5. 5
   기타to afford a beige solid
6. 6
   여과were collected by suction filtration
7. 7
   세척washed with water (200 mL)
8. 8
   기타dried in vacuo

실험 절차

Sulfated platinum (˜0.1 eq, 1 g) was added to a suspension of 6-chloro-4-fluoro-8-nitro-9H-β-carboline (1.0 eq, 35 mmol, 9.3 g) and ammonium formate (3.0 eq, 105 mmol, 6.6 g) in ethanol (175 mL) and the resulting mixture heated at 75° C. for 4 h. After cooling to RT the mixture was filtered through a short plug of Celite® washing with copious amounts of methanol, and then the filtrate concentrated in vacuo to afford a beige solid. The solid was suspended in the minimum volume of methanol and added dropwise to a vigorously stirred mixture of saturated sodium bicarbonate solution and saturated sodium chloride solution. After stirring for 15 min the precipitated solids were collected by suction filtration, washed with water (200 mL) and dried in vacuo to afford 6-chloro-4-fluoro-9H-β-carbolin-8-ylamine (5.8 g, 70% 2 steps) as a beige powder.

출처