Реакция #1256769

ord-07baa239dfbb4c0dbda1d0ce5446d3e4

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    ДругоеWhite crystals precipitated
  2. 2
    Фильтрацияwere collected by filtration
  3. 3
    Промывкаwashed with H2O (30 ml)
  4. 4
    ДругоеThe product was dried 1 h at 50° C. on the high vacuum
  5. 5
    Другоеto yield 9.25 g (84%) of a off white solid

Методика

4-Chloro-pyridine-3-carbaldehyde (10.0 g, 71 mmol) was dissolved in EtOH (12 ml). H2O (30 ml), ice (30 g) and hydroxylamine hydrochloride (5.40 g, 78 mmol) were added. To the resulting mixture was added over a period of 2 min a solution of 2 N NaOH (88.3 ml, 177 mmol). The resulting yellowish solution was stirred 2.5 h at r.t. before neutralisation with AcOH (pH=6). White crystals precipitated, were collected by filtration and washed with H2O (30 ml). The product was dried 1 h at 50° C. on the high vacuum to yield 9.25 g (84%) of a off white solid. m/z=157.1 ([M−H]−).

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US07825123B2uspto-grants-2010_11