HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium methanethiolate → 5-Acetyl-3-chloro-2-methylthiopyridine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium methanethiolate | HCID 4378561 | — |
| Reactant | 1-(5,6-Dichloropyridin-3-yl)ethan-1-one | HCID 10198006 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Solvent | tert-Butanol | HCID 6386 | — |
| Product | 5-Acetyl-3-chloro-2-methylthiopyridine | HCID 18435802 | 94% |
Reaction Steps
5-Acetyl-2,3-dichloropyridine (24.5 g, 0.129 mol) was slurried in t-butanol (200 mL) and sodium methanethiolate (10 g, 0.143 mol) was added. The mixture was heated under reflux conditions for two hours, cooled to room temperature, and diluted with water (200 mL) and ether (150 mL). This was separated and the aqueous phase extracted with ether (50 mL). The combined organic extracts were washed with water (100 mL) and saturated sodium chloride solution (100 mL), dried over anhydrous sodium sulphate, and evaporated to dryness to give the desired product (24.1 g, 94%) as a pale, low melting solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06436963B1 |
| Source dataset | uspto-grants-2002_08 |
| ORD ID | ord-23c56eaf6b234f50b4d908973966e4aa |
| Source note | uspto-grants-2002_08 |