HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diethyl Ether → HCID 19828389, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diethyl Ether | HCID 3283 | — |
| Reactant | Tributylphosphine | HCID 13831 | — |
| Reactant | 5-(Bromomethyl)-2-[(4-nitrophenyl)sulfanyl]pyridine-3-carbonitrile | HCID 13912551 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 19828389 | HCID 19828389 | — |
Reaction Steps
Alternatively, 3-cyano-2-(4-nitrophenylthio)-5-bromomethylpyridine is allowed to react in tetrahydrofuran with tri-(n-butyl)phosphine for ten hours. Following the addition of ether, the solid which forms is collected by filtration and washed with 1:1 tetrahydrofuran:ether to yield [3-cyano-2-(4-nitrophenylthio)pyridin-5-ylmethyl]-tri-(n-butyl)phosphonium bromide as a white solid; mp 175°-176° C.; NMR (CDCl3, 80 MHz) d 0.85-2.63 (m, 27H), 4.76 (d, 2H, J=15.4 Hz), 7.74 (d, 2H, J=9.0 Hz), 8.26 (d, 2H, J=9.0 Hz), 8.55 (brs, 1H), 8.79 (brs, 1H); IR (KBr) 2950, 2860, 2220, 1595, 1575, 1515, 1390, 1340, 1075 and 845 cm-1 ; HRMS 471.2116 (M+ -HBr), Calc'd. for C25H34N3O2PS471.2109.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04684653 |
| Source dataset | uspto-grants-1987_08 |
| ORD ID | ord-30c38e6c44134c8aa3772aafb891d2a6 |
| Source note | uspto-grants-1987_08 |