HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triphenylphosphine → 6-(2-Acetylthioethyl)-2-pyridylamine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triphenylphosphine | HCID 11776 | — |
| Reactant | ethyl N-ethoxycarbonyliminocarbamate | HCID 220568 | — |
| Reactant | HCID 12071474 | HCID 12071474 | — |
| Reactant | HCID 178418634 | HCID 178418634 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | 6-(2-Acetylthioethyl)-2-pyridylamine | HCID 21265855 | — |
Reaction Steps
Triphenyl phosphine (2.36 g) was dissolved in tetrahydrofuran (40 ml). To the solution was added, at −20° C., diethyl azodicarboxylate (1.56 g). The mixture was stirred for 5 minutes, to which was added a solution of 2-(6-amino-2-pyridyl)ethanol (0.62 g) in tetrahydrofuran (2 ml). The mixture was stirred for one minutes, to which was added thioacetic acid (0.64 ml), followed by stirring for 4 hours at 25° C. The reaction mixture was concentrated under reduced pressure. The concentrate was purified by means of a column chromatography (carrier: silica gel, 120 g, developing solvent: ethyl acetate-hexane, 2:1) to give the title compound (0.56 g), m.p.55-59° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06174877B1 |
| Source dataset | uspto-grants-2001_01 |
| ORD ID | ord-a071540fdb2843128c986b1d4ff25993 |
| Source note | uspto-grants-2001_01 |