反应 #40480

ord-99de42632e8e4623a5dd2ee602d10fb0

反应条件

温度
60°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

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

实验过程

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%).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07727985B2uspto-grants-2010_06