Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Propyl mercaptan | HCID 7848 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | 2,3-Dichloro-5-(trifluoromethyl)pyridine | HCID 112234 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 10999654 | HCID 10999654 | 99.4% |
Reaction Steps
23.8 g (0.313 mol) of 1-propanethiol were added in the course of 30 minutes to a mixture of 7.9 g (0.313 mol) of 95% pure sodium hydride in 200 ml of THF while flushing with nitrogen and stirring, a temperature of 25-30° C. being maintained by means of cooling. After the mixture had been stirred for 1 hour, 54 g (0.25 mol) of 2,3-dichloro-5-trifluoromethylpyridine in 50 ml THF were added at 25-30° C. in the course of 20 minutes with stirring, and stirring was continued for 10 hours at 23° C. The reaction mixture was concentrated in vacuo, taken up in methylene chloride, extracted with 0.5 N sodium hydroxide solution, dried over magnesium sulfate and concentrated, yielding 63.5 g (99.4%) of the title compound of nD23=1.5120.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06262273B1 |
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| Source dataset | uspto-grants-2001_07 |
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| ORD ID | ord-d6c3a044829f433bbec9951756089fa2 |
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| Source note | uspto-grants-2001_07 |
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