Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 3-(Chloromethyl)pyridine hydrochloride | HCID 23394 | — |
| Reactant | HCID 19771874 | HCID 19771874 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 131717424 | HCID 131717424 | 29.1% |
Reaction Steps
A solution of 3-picolyl chloride hydrochloride (2.50 g) and 3,6-dihydro-4-phenyl-1(2H)-pyridineethanethiol hydrochloride (3.90 g) (Example A) in 100 mL of dimethylformamide is treated with triethylamine (7.4 ml) and the mixture is heated at 80° C. for 8 hours. The solvent is evaporated in vacuo, and the residue is partitioned into chloroform/sodium bicarbonate solution. The organic extract is dried over magnesium sulfate, filtered and concentrated. The crude product is purified by column chromatography (silica gel; 2% methanol in chloroform) to yield 1.7 g of the title compound as an oil, which is converted into its hydrochloride salt (hydrogen chloride gas in diethyl ether) and recrystallized from ethanol/acetonitrile; mp 218°-220° C. (dec).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05120748 |
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| Source dataset | uspto-grants-1992_06 |
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| ORD ID | ord-5583e05ea6a149208541f556327f8141 |
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| Source note | uspto-grants-1992_06 |
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