HuagongsheHuagongshe Chemistry Print Report · For research reference only
Pyridine → HCID 18786088, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Pyridine | HCID 1049 | — |
| Reactant | Acryloyl chloride | HCID 13140 | — |
| Reactant | HCID 18786085 | HCID 18786085 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 18786088 | HCID 18786088 | 81% |
Reaction Steps
A suspension of 89 g (0.19 mol) of [(2-amino-4-fluorophenyl)methyl]-triphenylphosphonium bromide in 1.5 L CH2Cl2 was stirred and 17 mL (0.21 mol) of acryloyl chloride was added dropwise. A 22.8 mL sample of pyridine was added dropwise. The mixture was heated under reflux for 45 min. The mixture was cooled, washed with K2CO3 solution, dilute hydrochloric acid and brine. It was dried (Na2SO4), concentrated and triturated with Et2O to give 80 g (81%) of [[4-fluoro-2-[(1-oxo-2-propenyl)amino]phenyl]methyl]triphenylphosphonium bromide as a yellowish solid: 1H NMR (CDCl3) δ 8.0-7.4 (m, 15H); 6.9 (m, 2H); 6.4 (m, 1H); 6.1 (d, 1H); 5.9 (d, 2H); 5.5 (d, 1H). ##STR18##
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06063803 |
| Source dataset | uspto-grants-2000_05 |
| ORD ID | ord-8f7d112b6a1b4b9eb7ffa85821a68179 |
| Source note | uspto-grants-2000_05 |