HuagongsheHuagongshe Chemistry Print Report · For research reference only
Di-tert-butyl peroxide → HCID 15169992, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Di-tert-butyl peroxide | HCID 8033 | — |
| Reactant | 1-Hydroxy-4-benzoyloxy-2,2,6,6-tetramethylpiperidine | HCID 688178 | — |
| Reactant | HCID 15169991 | HCID 15169991 | — |
| Solvent | 1,2-Dichlorobenzene | HCID 7239 | — |
| Product | HCID 15169992 | HCID 15169992 | 5.2% |
Reaction Conditions
| Temperature | 135 °C |
|---|
Reaction Steps
A mixture of 43.6 grams (122 mmol) of the compound prepared in Example 21A, 40.5 grams (147 mmol) of 4-benzoyloxy-1-oxyl-2,2,6,6-tetramethylpiperidine, 17.8 grams (122 mmol) of di-tert-butyl peroxide and 50 ml of 1,2-dichlorobenzene is heated at 135° C. for 5.5 hours in a Fisher-Porter pressure bottle. Fresh di-tert-butyl peroxide (8.0 grams, 55 mmol) is added and the reaction mixture is heated at 135° C. for an additional three hours. The crude reaction mixture is purified by flash chromatography on silica gel (hexane; then 100:3 heptane:ethyl acetate) to afford 4.0 grams of the title compound as a while solid melting at 140°-142° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05442071 |
| Source dataset | uspto-grants-1995_08 |
| ORD ID | ord-aaec8a4efca24034a1441fc8a9ace29a |
| Source note | uspto-grants-1995_08 |