反应 #61377

ord-928dcbd36ef14c3e9a91d1edde5a98fa

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    workup.STIRRINGstirring
  2. 2
    workup.WAITcontinued for another 24 hours
  3. 3
    洗涤was then washed with a 2% sodium hydroxide (w/w) solution until no p-nitrophenol
  4. 4
    干燥The dichloromethane was dried with sodium sulfate
  5. 5
    过滤filtered
  6. 6
    其他evaporated under reduced pressure

实验过程

To a stirring slurry of 9-anthracenemethanol (10 g, 48 mmol) and 4-nitrophenyl chloroformate (13.6 g, 67.5 mmol) in 200 ml CH2Cl2 was added triethylamine (6.7 ml, 0.19 mol). The resulting gold colored solution was allowed to stir 16 hrs at room temperature. At this point, 2-(2-aminoethoxy)ethanol (14.4 ml, 0.144 mol) was added and stirring continued for another 24 hours. The CH2Cl2 reaction mixture was then washed with a 2% sodium hydroxide (w/w) solution until no p-nitrophenol was observed in the organic layer. The dichloromethane was dried with sodium sulfate, filtered, and evaporated under reduced pressure.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07429472B2uspto-grants-2008_09