HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sulfuric Acid → 2,2,6,6-Tetramethyl-4-hydroxy-4-tert.-butylcarbamoyl piperidine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sulfuric Acid | HCID 1118 | — |
| Reactant | tert-Butanol | HCID 6386 | — |
| Reactant | 4-Piperidinecarbonitrile, 4-hydroxy-2,2,6,6-tetramethyl- | HCID 90874 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Product | 2,2,6,6-Tetramethyl-4-hydroxy-4-tert.-butylcarbamoyl piperidine | HCID 20303341 | — |
Reaction Steps
54.6 g 2,2,6,6-Tetramethyl-4-hydroxy-4-cyanopiperidine together with 45 g tert.-butanol in 200 ml glacial acetic acid are introduced into the reactor. Subsequently, 60 g concentrated sulfuric acid are added dropwise with agitation, and agitation is continued for 2 hours at 70° C., thus forming a precipitate which is filtered off and dissolved in water. On alkalization with NaOH, the product precipitates, it is suction-filtered and recrystallized from ethyl acetate. Yield 44 g, m.p. 134°-136° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04239891 |
| Source dataset | uspto-grants-1980_12 |
| ORD ID | ord-deeb7a32d54b48fea464100efeb985de |
| Source note | uspto-grants-1980_12 |