Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | 1,4-Dihydroxy-2,2,6,6-tetramethylpiperidine | HCID 5395 | — |
| Solvent | Isopropanol | HCID 3776 | — |
| Product | 4972-11-6 | HCID 66868295 | — |
Reaction Steps
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.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US06254724B1 |
|---|
| Source dataset | uspto-grants-2001_07 |
|---|
| ORD ID | ord-856f89c04d11431589f7c61e0390d63e |
|---|
| Source note | uspto-grants-2001_07 |
|---|