Реакция #155720

ord-105a12909b6245179ca0ecfa4091af6a

Растворители

Условия реакции

Температура
0°CELSIUS
Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    ТемператураThe mixture was warmed up
  2. 2
    Другоеto react
  3. 3
    Температураunder reflux for 2 h
  4. 4
    ДругоеAfter completion of the reaction
  5. 5
    Фильтрацияfiltered by suction
  6. 6
    ПромывкаThe filtered cake was washed with water and petroleum ether
  7. 7
    Другоеdried

Методика

Intermediate b (21 g, 0.08 mol) and anhydrous sodium acetate (29 g, 0.35 mol) were added to glacial acetic acid (20v/w, 420 mL). The mixture was warmed up to react under reflux for 2 h. After completion of the reaction, the reaction solution was cooled to 0° C. and poured into water (1200 mL). The mixture was stirred for 30 min and filtered by suction. The filtered cake was washed with water and petroleum ether, and dried to produce an orange red solid (12 g) in a yield of 67.8%.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US08822465B2uspto-grants-2014_09