HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Hydroxide → 5-Ethynylpyridin-2-amine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 67000911 | HCID 67000911 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | 5-Ethynylpyridin-2-amine | HCID 21954827 | 36.4% |
Reaction Steps
A solution of 4-(6-amino-pyridin-3-yl)-2-methyl-but-3-yn-2-ol (example D.1 method 2 step 1) (22.5 g, 128 mmol) in toluene (500 mL) was refluxed in the presence of powdered NaOH (3.83 g, 96 mmol) for 16 h. The solvent was removed under reduced pressure to leave a brown residue which was purified by silica gel column chromatography with dichloromethane and ether, followed by trituration with heptane to give the title compound (5.5 g, 36%) (31.1 g, 100%) as light red solid. MS (EI) 118.1 [(M)+]; mp 143° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07446113B2 |
| Source dataset | uspto-grants-2008_11 |
| ORD ID | ord-4b7a81f9be0544cba8c8152ccc629879 |
| Source note | uspto-grants-2008_11 |