HuagongsheHuagongshe Chemistry Print Report · For research reference only
2-Fluoro-6-methoxybenzonitrile → 2-Fluoro-6-hydroxybenzonitrile
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 2-Fluoro-6-methoxybenzonitrile | HCID 523101 | — |
| Reactant | Pyridinium chloride | HCID 10176127 | — |
| Product | 2-Fluoro-6-hydroxybenzonitrile | HCID 2783216 | 66.4% |
Reaction Steps
7.8 g of 2-methoxy-6-fluorobenzonitrile and 18.0 g of pyridine hydrochloride were heated for 5 hours at 195° C. under dry nitrogen. After cooling, the batch was partitioned between 50 ml of water and 50 ml of tert-butyl methyl ether, and the organic phase was subsequently extracted with 40 ml of 2N NaOH. The alkali extract was brought to pH 5 and subsequently extracted twice with in each case 40 ml of tert-butyl methyl ether. After the solvent had been evaporated, 4.7 g of the desired product were obtained as an oil (HPLC: 93%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06680402B2 |
| Source dataset | uspto-grants-2004_01 |
| ORD ID | ord-d54f9454a25c460694086778033ecf50 |
| Source note | uspto-grants-2004_01 |