HuagongsheHuagongshe Chemistry Print Report · For research reference only
Tributylphosphine → HCID 86615985, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Tributylphosphine | HCID 13831 | — |
| Reactant | 1,1'-(Azodicarbonyl)dipiperidine | HCID 73042 | — |
| Reactant | 2-Chloro-5-hydroxypyridine | HCID 819821 | — |
| Reactant | HCID 59518064 | HCID 59518064 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | HCID 86615985 | HCID 86615985 | 98.2% |
Reaction Steps
3-[4-(1-Hydroxy-4,4-dimethyl-pentyl)-benzoylamino]-propionic acid methyl ester (546 mg, 1.7 mmol) and 6-chloro-pyridin-3-ol (270 mg, 2.09 mmol) are combined in anhydrous toluene (10 mL), degassed, filled with nitrogen for 3 times, and cooled in an ice bath. Tributylphosphine (TBP) (630 uL, 2.55 mmol) is added to the reaction mixture under nitrogen at 0° C., followed by addition of 1,1′-(azodicarbonyl)-dipiperidine (ADDP) (643 mg, 2.55 mmol). The reaction mixture is allowed to warm to room temperature and stirred over night, the mixture is loaded on silica gel column. Chromatography gave the title compound (722 mg, 1.67 mmol).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08609892B2 |
| Source dataset | uspto-grants-2013_12 |
| ORD ID | ord-ad8e7b5ea2334f429478567ae67a1309 |
| Source note | uspto-grants-2013_12 |