HuagongsheHuagongshe Chemistry Print Report · For research reference only
Benzyl Alcohol → HCID 70653970, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Benzyl Alcohol | HCID 244 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | 2,6-Dichloroisonicotinic acid | HCID 94830 | — |
| Reactant | HCID 178418361 | HCID 178418361 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 70653970 | HCID 70653970 | — |
Reaction Steps
In an argon atmosphere, 2,6-dichloroisonicotinic acid (57.6 g) was gradually added to 55% sodium hydride (52.5 g) and dimethylformamide (1 L) while being cooled and stirred. Subsequently, benzyl alcohol (93 mL) was gradually added dropwise to the reaction product at the same temperature. After hydrogen was no longer generated, the reaction product was stirred for 4 hours at 80° C., and water (1 L) was then added thereto. The mixture was separated by a mixed solvent (1 L) of ethyl acetate and n-hexane (1:1). The acidity of the aqueous layer was lowered with acetic acid (75.5 mL), and water (1.7 L) was further added thereto. The precipitate was filtered and dried to obtain Compound 2a.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08889699B2 |
| Source dataset | uspto-grants-2014_11 |
| ORD ID | ord-538b8bd398b14de7bb79a705935706e1 |
| Source note | uspto-grants-2014_11 |