Реакция #59516

ord-eb11651813c84c2689f6df85f5f39bf2

Растворители

Условия реакции

Температура
90°CELSIUS
Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    ДругоеReaction mixture
  2. 2
    ДругоеReaction mixture
  3. 3
    Температураwas cooled
  4. 4
    workup.ADDITIONAfter addition reaction mixture
  5. 5
    Температураwas heated at 60° C. for an hour
  6. 6
    ФильтрацияPrecipitate was filtered
  7. 7
    Промывкаwashed with water

Методика

Triethylamine was added to solution of p-anisaldehyde (10 g) and phenylacetic acid (10 g) in acetic anhydride (25 ml). Reaction mixture was stirred at 90° C. for 8 h. Reaction mixture was cooled and water (600 ml) solution of potassium carbonate (81 g) was added. After addition reaction mixture was heated at 60° C. for an hour. Before neutralising with concentrated hydrochloric acid the reaction mixture was cooled below 10° C. Precipitate was filtered and washed with water. 1H-NMR (400 MHz, d6-DMSO): 12.6 (bs, 1H), 7.67 (s, 1H), 7.4-7.3 (m, 3H), 7.2-7.1 (m, 2H), 7.0-6.9 (m, 2H), 6.8-6.7 (m, 2H), 3.70 (s, 3H). (M)+=254 (100%).

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US07425568B2uspto-grants-2008_09