HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → Methyl 2-chloro-6-methoxyisonicotinate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | Methyl 2,6-dichloroisonicotinate | HCID 93237 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Solvent | Ammonium Chloride | HCID 25517 | — |
| Product | Methyl 2-chloro-6-methoxyisonicotinate | HCID 13339618 | — |
Reaction Steps
To a solution of dry methanol (2.2 mL, 53 mmol) in THF (200 mL) was added sodium hydride (2.12 g, 53 mmol) in portions under a stream of nitrogen. When gas evolution ceased, 2,6-dichloro-isonicotinic acid methyl ester (10.0 g, 48.5 mmol) was added. After stirring for 2 hours, the reaction was diluted with saturated aqueous ammonium chloride (100 mL) and extracted with ethyl acetate (4×50 mL). The combined organics were washed with brine, dried over sodium sulfate, and concentrated to afford 2-chloro-6-methoxy-isonicotinic acid methyl ester.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08063065B2 |
| Source dataset | uspto-grants-2011_11 |
| ORD ID | ord-22b412909e3a4838953bbd1eb09163e4 |
| Source note | uspto-grants-2011_11 |