HuagongsheHuagongshe Chemistry Print Report · For research reference only
Toluene → HCID 23113966, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Toluene | HCID 1140 | — |
| Reactant | Triphenylphosphine | HCID 11776 | — |
| Reactant | ethyl N-ethoxycarbonyliminocarbamate | HCID 220568 | — |
| Reactant | HCID 23114180 | HCID 23114180 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 23113966 | HCID 23113966 | 84% |
Reaction Steps
To a solution of 2-(2-hydroxy-1-(4-isopropylphenyl)ethyl)-3,5,6-trimethylphenol obtained in Reference Example 8 (7.85 g, 26.3 mmol) and triphenylphosphine (7.58 g, 28.9 mmol) in THF (60 mL) was added diethyl azodicarboxylate (a 40% toluene solution, 12.6 g, 28.9 mmol) with ice-cooling, and the mixture was stirred at room temperature for 1 hour. The solvent was concentrated under reduced pressure to obtain the residue, which was purified by silica gel column chromatography (hexane:ethyl acetate=10:1) to obtain 5.70 g (yield 84%) of the title compound. Melting point: 48-49° C. (methanol).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07507841B2 |
| Source dataset | uspto-grants-2009_03 |
| ORD ID | ord-36071a950ced47cc9b3a73d604d452bd |
| Source note | uspto-grants-2009_03 |