Реакция #67941

ord-470fd18e4c004da9bf043eb5c0be01eb

Растворители

Условия реакции

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

Обработка

  1. 1
    ДругоеMost of the solvent was evaporated
  2. 2
    Фильтрацияthe precipitate was filtered
  3. 3
    Промывкаwashed with Et2O
  4. 4
    ДругоеDrying under hv

Методика

The aforementioned mixture of amides 14a/14b (500 mg, 1.43 mmol) was suspended in glacial acetic acid (8 mL) and heated to 90° C. for 7 h. Most of the solvent was evaporated, and the yellow residue was suspended in Et2O. After being vigorously stirred for 20 min, the precipitate was filtered and washed with Et2O. Drying under hv gave 404 mg (85%) of 15 as a beige solid. Data of 15: Rf 0.80 (hexane/EtOAc 1:5). 1H NMR (300 MHz, DMSOd6): δ 3.76 (s, 3H), 4.14 (s, 3H), 4.34 (s, 3H), 7.14-7.17 (m, 1H), 7.48-7.55 (m, 3H), 8.25 (s, 1H). MS (ESI): m/z (rel intensity) 331 (98).

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US08524899B2uspto-grants-2013_09