反応 #684974

ord-90661967ac1541b688649dc2500118ba

反応方程式

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
収率 84.1%
Oc1cccnc1Cc1ccc(Br)cc1F
2-(4-Bromo-2-fluorobenzyl)-3-pyridinol
収率 84.1%

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.ADDITIONwas added
  2. 2
    洗浄The ethyl acetate layer was washed with saturated brine
  3. 3
    濃縮concentrated under reduced pressure
  4. 4
    その他The residue was purified by silica gel column chromatography

実験手順

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).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07897387B2uspto-grants-2011_03