Реакция #1470427

ord-856f89c04d11431589f7c61e0390d63e

Реагенты

Нет

Растворители

Условия реакции

Температура
20°CELSIUS
Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Температураby occasionally cooling with an ice bath
  2. 2
    Фильтрацияfiltered
  3. 3
    Промывкаwashed with isopropanol
  4. 4
    Другоеgiving a pale yellow solid
  5. 5
    Другое5.0 g of this crude product is recrystallized from 100 mL isopropanol affording 3 g of a white crystalline solid, mp>260° C.

Методика

67 mL of isopropanol is cooled to 0° C. and saturated with HCl gas. This solution is added dropwise to a mechanically stirred solution of 50 g (0.29 mol) 1-oxyl-2,2,6,6-tetramethyl-4-hydroxypiperidine in 130 mL of isopropanol, maintaining a reaction temperature of about 20° C. by occasionally cooling with an ice bath. The HCl salt is vacuum filtered and washed with isopropanol, giving a pale yellow solid. 5.0 g of this crude product is recrystallized from 100 mL isopropanol affording 3 g of a white crystalline solid, mp>260° C.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US06254724B1uspto-grants-2001_07