HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetone → 2-(5-Bromopyridin-2-yl)propan-2-ol
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetone | HCID 180 | — |
| Reactant | 2,5-Dibromopyridine | HCID 69353 | — |
| Reactant | Butyllithium | HCID 178418339 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | 2-(5-Bromopyridin-2-yl)propan-2-ol | HCID 15486392 | 86% |
Reaction Steps
2,5-Dibromopyridine (1.04 g, 4.39 mmol) was dissolved in toluene (22 mL) in a 100 mL round-bottomed flask. The mixture was cooled to −78° C. n-Butyllithium (3.02 mL, 4.83 mmol) was added dropwise. The mixture was stirred 30 min, followed by the addition of acetone (2 mL). The mixture was stirred 40 min and then let warm to rt. The mixture was washed with ammonium chloride (5% aq, 50 mL), water (50 mL) and then brine (50 mL). The organic layer was dried over sodium sulfate, filtered and concentrated. The residue was purified by Biotage (16% ethyl acetate in hexanes). Concentration of the desired fractions afforded the product (0.82 g, 3.78 mmol, 86% yield). MS (ESI) m/z 216.0 [M]+, 218.1 [M+2]+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09193692B2 |
| Source dataset | uspto-grants-2015_11 |
| ORD ID | ord-1704597e4a514dd6ab25adbab1caab2f |
| Source note | uspto-grants-2015_11 |