تفاعل #684974

ord-90661967ac1541b688649dc2500118ba

معادلة التفاعل

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

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

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

الإجراء التجريبي

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).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07897387B2uspto-grants-2011_03