반응 #684974

ord-90661967ac1541b688649dc2500118ba

반응 방정식

CCOC(C)=O
ethyl acetate
O=C(O)C(F)(F)F
Trifluoroacetic acid
COCOc1cccnc1Cc1ccc(Br)cc1F
compound
COCOc1cccnc1Cc1ccc(Br)cc1F
2-(4-Bromo-2-fluorobenzyl)-3-(methoxymethoxy)pyridine
O=C([O-])O.[Na+]
sodium hydrogencarbonate
Oc1cccnc1Cc1ccc(Br)cc1F
title compound
수율 84.1%
Oc1cccnc1Cc1ccc(Br)cc1F
2-(4-Bromo-2-fluorobenzyl)-3-pyridinol
수율 84.1%

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.ADDITIONwas added
  2. 2
    세척The ethyl acetate layer was washed with saturated brine
  3. 3
    농축concentrated under reduced pressure
  4. 4
    기타The residue was purified by silica gel column chromatography

실험 절차

Trifluoroacetic acid (1 ml) was added to the compound of Example B244 (134 mg, 0.411 mmol) in methylene chloride (4 ml), and this reaction mixture was stirred at room temperature overnight. After neutralizing the mixture with saturated aqueous sodium hydrogencarbonate, ethyl acetate was added. The ethyl acetate layer was washed with saturated brine and concentrated under reduced pressure. The residue was purified by silica gel column chromatography to give the title compound (97.5 mg).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07897387B2uspto-grants-2011_03