HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diethyl Ether → HCID 178512256, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diethyl Ether | HCID 3283 | — |
| Reactant | 5-Amino-2-chloropyridine | HCID 79305 | — |
| Reactant | Diphenyl N-Cyanocarbonimidate | HCID 688090 | — |
| Reactant | Chloroform methanol | HCID 21584188 | — |
| Solvent | Ethylene | HCID 6325 | — |
| Product | HCID 178512256 | HCID 178512256 | 95.7% |
Reaction Steps
A stirred mixture of 5-amino-2-chloropyridine (1.3 g, 0.01 mol) and diphenylcyanocarbonimidate (2.4 g, 0.01 mol) in 15 ml of ethylene glycoldimethyl ether (DME), under nitrogen, was kept at 60° C. for 24 hours and at 85° C. for 6 hours when it was allowed to cool to room temperature. The solvent was removed in vacuo and the residue was heated to a melt at 120° C., under nitrogen, for 1 hour to complete the reaction as shown by TLC (5% MeOH/CHCl3). This was allowed to cool and was triturated with Et2O to give a solid that was collected by filtration. The solid was washed with Et2O to give 2.61 g of the titled product.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05567722 |
| Source dataset | uspto-grants-1996_10 |
| ORD ID | ord-fe2c592282ad4818ae8d76cea7922209 |
| Source note | uspto-grants-1996_10 |