反应 #1470427

ord-856f89c04d11431589f7c61e0390d63e

反应方程式

Cl
HCl
CC1(C)CC(O)CC(C)(C)N1O
1-oxyl-2,2,6,6-tetramethyl-4-hydroxypiperidine
Cl
HCl
CC1(C)CC(O)CC(C)(C)[NH+]1O.[Cl-]
1-Hydroxy-2,2,6,6-tetramethyl-4-hydroxypiperidinium Chloride

反应条件

温度
20°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度by occasionally cooling with an ice bath
  2. 2
    过滤filtered
  3. 3
    洗涤washed with isopropanol
  4. 4
    其他giving a pale yellow solid
  5. 5
    其他5.0 g of this crude product is recrystallized from 100 mL isopropanol affording 3 g of a white crystalline solid, mp>260° C.

实验过程

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.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US06254724B1uspto-grants-2001_07