반응 #428749

ord-3d1c8c674c9949dca91664f1b2560a93

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.STIRRINGstirring
  2. 2
    workup.WAITcontinued for another 24 hours
  3. 3
    세척was then washed with a 2% sodium hydroxide (w/w) solution until no p-nitrophenol
  4. 4
    건조The dichloromethane was dried with sodium sulfate
  5. 5
    여과filtered
  6. 6
    기타evaporated under reduced pressure

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08895787B2uspto-grants-2014_11