HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 68559388, compound → 6-Difluoromethyl-2-(3-methoxy-propyl)-nicotinic acid methyl ester
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 68559388 | HCID 68559388 | — |
| Reactant | HCID 178418361 | HCID 178418361 | — |
| Catalyst | Palladium | HCID 23938 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Triethylamine | HCID 8471 | — |
| Product | 6-Difluoromethyl-2-(3-methoxy-propyl)-nicotinic acid methyl ester | HCID 68560737 | 113.4% |
Reaction Steps
A solution of 194 g of 6-(Chloro-difluoro-methyl)-2-(3-methoxy-propyl)-nicotinic acid methyl ester (prepared according to WO 04/078729) in methanol (ca. 2 liter) and triethylamine (100 ml) is hydrogenated at 1 Atm hydrogen pressure in the presence of 2 g of 5% palladium supported on carbon. After completion of the reduction the reaction mixture is filtered through hyflo, and the filtrate diluted with water and the water/methanol mixture then extracted with ethyl acetate. The combined ethyl acetate extracts are washed with saturated aqueous sodium chloride solution, dried over magnesium sulphate and then concentrated in vacuo to give 194.2 g 6-Difluoromethyl-2-(3-methoxy-propyl)-nicotinic acid methyl ester as a pale coloured oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07745495B2 |
| Source dataset | uspto-grants-2010_06 |
| ORD ID | ord-42fb344170e94a92985abc60d64e31f2 |
| Source note | uspto-grants-2010_06 |