Реакция #309254

ord-116db555946d4209aa66ef0278629dfe

Реагенты

Нет

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Фильтрацияwas filtered off
  2. 2
    workup.ADDITIONSolid Na2CO3 was added to the solution
  3. 3
    workup.STIRRINGstirred for additional 10 min
  4. 4
    ФильтрацияThe solid was filtered off
  5. 5
    Концентрированиеthe solution was concentrated
  6. 6
    ДругоеPurification on a silica gel column

Методика

To a solution of 4-bromophenol (0.50 g, 2.89 mmol) and dimethoxymethane (2.6 mL, 29.39 mmol) in DCM (60 mL) was added P2O5 (1.50 g, 10.57 mmol). The reaction mixture was stirred at for 1 h and insoluble precipitate was filtered off. Solid Na2CO3 was added to the solution and stirred for additional 10 min. The solid was filtered off and the solution was concentrated. Purification on a silica gel column gave the desired product as a clear oil (363 mg). NMR (CDCl3): 7.38 (d, 2H), 6.93 (d, 2H), 5.15 (s, 2H), 3.47 (s, 3H).

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US08207178B2uspto-grants-2012_06