Реакция #6910

ord-410a6f1443c34331ba6735f7cc64c911

Растворители

Условия реакции

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

Обработка

  1. 1
    Промывкаwashed twice with brine
  2. 2
    Сушкаdried over sodium sulfate
  3. 3
    Фильтрацияfiltered through a fritted funnel
  4. 4
    Другоеthe volatiles were removed under vacuum
  5. 5
    ДругоеThis provided the product, MS
  6. 6
    Другоеm/z 356, which was used in the next step without further purification

Методика

A mixture of the product of Step D (60 mg; 0.1863 mmol), hydroxyl amine hydrochloride (3 eq.), sodium carbonate (4 eq.) in 1.5 mL water and 2.5 mL ethanol was heated to 90° C. for 6 h. The mixture was diluted with dichloromethane, washed twice with brine, dried over sodium sulfate, filtered through a fritted funnel and the volatiles were removed under vacuum. This provided the product, MS: m/z 356, which was used in the next step without further purification.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US07084156B2uspto-grants-2006_08