반응 #2006442

ord-847a1d33b4cf43d084f625e651ea099f

반응 방정식

NCCOCCO
2-(2-aminoethoxy)ethanol
OCc1c2ccccc2cc2ccccc12
9-anthracenemethanol
O=C(Cl)Oc1ccc([N+](=O)[O-])cc1
4-nitrophenyl chloroformate
CCN(CC)CC
triethylamine
O=C(NCCOCCO)OCc1c2ccccc2cc2ccccc12
[2-(2-Hydroxy-ethoxy)-ethyl]-carbamic acid anthracen-9-ylmethyl ester

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: US08168405B2uspto-grants-2012_05