反応 #40480

反応方程式

charcoal

6-chloro-7-ethylsulfanyl-8-nitro-9H-β-carboline

ammonium chloride

→

6-chloro-7-ethylsulfanyl-9H-β-carbolin-8-ylamine

収率 100.0%

溶媒

ethyl acetate

ethanol

反応条件

後処理

1. 1
   温度Next, the mixture was cooled to RT
2. 2
   workup.ADDITIONwas added
3. 3
   ろ過The resulting mixture was filtered through a pad of celite
4. 4
   濃縮the filtrate was concentrated

実験手順

A 50 ml round-bottom flask with magnetic stirrer was charged with 6-chloro-7-ethylsulfanyl-8-nitro-9H-β-carboline (85.0 mg, 0.28 mmol) in 10 ml anhydrous ethanol. To the resulting orange mixture at RT was added 0.33 M aqueous ammonium chloride (2.0 ml, 0.66 mmol) and iron powder (680 mg, 12.2 mmol). The reaction mixture was heated to 60° C. and stirred vigorously for 20 hr. Next, the mixture was cooled to RT, diluted with ethyl acetate (15 ml), and activated charcoal (˜180 mg) was added. The resulting mixture was filtered through a pad of celite and the filtrate was concentrated to afford 77.8 mg of 6-chloro-7-ethylsulfanyl-9H-β-carbolin-8-ylamine as a yellow solid (>99%).

出典