反应 #1435682

ord-84ea0ca979854fbdb360bb8afb5c4e89

反应方程式

Cl
HCl
COc1c(C)cc([N+](=O)[O-])cc1[N+](=O)[O-]
2,4-dinitro-6-methylanisole
CCO
ethanol
[H][H]
hydrogen
COc1c(C)cc(N)cc1N.Cl.Cl
2,4-Diamino-6-methylanisole dihydrochloride

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度Subsequently, the mixture was cooled
  2. 2
    过滤The catalyst was filtered off
  3. 3
    其他the filtrate was evaporated to dryness on a rotary evaporator
  4. 4
    萃取The residue was extracted
  5. 5
    过滤filtered off
  6. 6
    其他dried overnight under reduced pressure

实验过程

105 g of 2,4-dinitro-6-methylanisole, 1.35 l of ethanol, 150 ml of water and 1 g of Pd/C (5% strength) were initially introduced into the autoclave and hydrogenated at 50° C. with a hydrogen pressure of 50 bar for 12 h. Subsequently, the mixture was cooled and then poured into 1.0 l of semiconcentrated HCl. The catalyst was filtered off, and the filtrate was evaporated to dryness on a rotary evaporator. The residue was extracted by boiling with 2×150 ml of ethanol, filtered off and dried overnight under reduced pressure.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07211119B2uspto-grants-2007_05