반응 #2045035

ord-b2d373b25ed84322810d7490682acdcc

반응 방정식

CC(Oc1ccc([N+](=O)[O-])cc1)C(=O)O
2-(4-Nitro-phenoxy)-propionic acid
OCCO
ethylene glycol
Cl
HCl
CC(Oc1ccc([N+](=O)[O-])cc1)C(=O)OCCO
48
수율 56.8%
CC(Oc1ccc([N+](=O)[O-])cc1)C(=O)OCCO
2-(4-Nitro-phenoxy)-propionic acid 2-hydroxy-ethyl ester
수율 56.8%

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타for 1½ hours
  2. 2
    기타During HCl gas bubbling the temp
  3. 3
    기타rose to 60° C
  4. 4
    기타The crude reaction mass
  5. 5
    추출Crude 48 was extracted into chloroform
  6. 6
    건조dried over Na2SO4
  7. 7
    workup.DISTILLATIONdistilled
  8. 8
    기타purified by column chromatography on silica gel

실험 절차

To a mixture of 2-(4-Nitro-phenoxy)-propionic acid 47 (45 g, 213 mol) and ethylene glycol (135 ml) was passed dry HCl gas for 1½ hours. During HCl gas bubbling the temp. rose to 60° C. The crude reaction mass was poured onto cold water (600 ml). Crude 48 was extracted into chloroform, dried over Na2SO4, distilled and purified by column chromatography on silica gel using hexane as eluant to give pure 48 (28 g, 56.8%) as a syrup.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08409559B2uspto-grants-2013_04