HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → 2-(4-Chloro-3,5-dimethoxyphenyl)-4-hydroxymethylpyridine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Ethyl chloroformate | HCID 10928 | — |
| Reactant | 2-(4-Chloro-3,5-dimethoxyphenyl)isonicotinic acid | HCID 22558039 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | 2-(4-Chloro-3,5-dimethoxyphenyl)-4-hydroxymethylpyridine | HCID 22557971 | — |
Reaction Steps
To an ice-cooled solution of 2-(4-chloro-3,5-dimethoxyphenyl)isonicotinic acid (7.20 g) and triethylamine (5.6 mL) in THF (70 mL) was added ethyl chloroformate (2.8 mL). The mixture was stirred at room temperature for 1 hour and filtered. To the filtrate was then added a solution of sodium borohydride (1.25 g) in water (4 mL). The mixture was stirred at room temperature for another hour and evaporated. Water was added to the residue and extracted with chloroform. The organic layer was washed with brine, dried over anhydrous sodium sulfate and evaporated. The residue was subjected to silica gel column chromatography using chloroform-methanol (20:1) and then chloroform-methanol (15:1) to give the title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06605620B1 |
| Source dataset | uspto-grants-2003_08 |
| ORD ID | ord-b857465a9ea74052be60ac31d64163f6 |
| Source note | uspto-grants-2003_08 |