Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | Picolyl chloride hydrochloride | HCID 23392 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | 2-Chlorobenzimidazole | HCID 78572 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 13423750 | HCID 13423750 | — |
Reaction Steps
61.0 g of 2-chlorobenzimidazole are first added at 25° C. to a suspension of 41.9 g of sodium hydride (55-60% dispersion) in 500 ml of dimethylformamide, and 66.0 g of 2-picolyl chloride-hydrochloride are then added. The mixture is stirred for 1 hour at room temperature and for a further 2 hours at 60° C. After dilution with 1 liter of ethyl acetate, 250 ml of water are carefully added dropwise, the phases are separated, and the ethyl acetate phase is concentrated in vacuo. The remaining product melts at 75°-77° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US04585775 |
|---|
| Source dataset | uspto-grants-1986_04 |
|---|
| ORD ID | ord-4f83a61e61b04569b74e0846428e53ae |
|---|
| Source note | uspto-grants-1986_04 |
|---|
