HuagongsheHuagongshe Chemistry Print Report · For research reference only
Tributylphosphine → HCID 67485984, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Tributylphosphine | HCID 13831 | — |
| Reactant | 1,1'-(Azodicarbonyl)dipiperidine | HCID 73042 | — |
| Reactant | 4-Bromo-3,5-dimethylphenol | HCID 81970 | — |
| Reactant | HCID 67486312 | HCID 67486312 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | HCID 67485984 | HCID 67485984 | — |
Reaction Steps
A solution of 4-bromo-3,5-dimethyl-phenol (818 mg, 4.07 mmol) and 3-[4-(1-hydroxymethyl-2-methyl-propyl)-benzoylamino]-propionic acid ethyl ester (1.0 g, 3.26 mmol) in anhydrous toluene (15 mL) is degassed and filled with nitrogen 3 times. Tributylphosphine (1.21 mL, 4.89 mmol) is added to the reaction mixture under nitrogen at 0° C., followed by addition of 1,1′-(azodicarbonyl)-dipiperidine (1.23 g, 4.89 mmol). The reaction mixture is allowed to warm to room temperature and stirred overnight. The mixture is loaded on a silica gel column and purified using hexanes/ethyl acetate. MS (ES): 488.2 [M+H]−.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08076374B2 |
| Source dataset | uspto-grants-2011_12 |
| ORD ID | ord-1eba1351470c4317801afa63f4ec304a |
| Source note | uspto-grants-2011_12 |