Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Methanethiol | HCID 878 | — |
| Reactant | Water | HCID 962 | — |
| Reactant | Potassium | HCID 5462222 | — |
| Reactant | HCID 13755201 | HCID 13755201 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 21292461 | HCID 21292461 | 98% |
Reaction Steps
A solution of 3.5 g (0.01 mol) of 5-bromo-1-(2-chloro-4-trifluoromethyl-phenyl)-4-cyano-pyrazole is added dropwise at 20°-25° C. to a suspension of 0.011 mol of potassium methylmercaptide, prepared by passing 0.6 g (0.011 mol) of methyl mercaptan into a solution of 1.4 g (0.012 mol) of potassium t-butylate in 50 ml of tetrahydrofuran. The mixture is stirred overnight, poured into water, and extracted by shaking three times with 100 ml of methylene chloride in each case. After drying the combined phases over sodium sulphate, the solution is concentrated in vacuo. An oily residue remains which crystallizes after standing overnight. 3.1 g (98% of theory) of 1-(2-chloro-4-trifluoromethyl-phenyl)-4-cyano-5-methylthio-pyrazole of melting point 59°-62° C. are obtained.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US04770692 |
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| Source dataset | uspto-grants-1988_09 |
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| ORD ID | ord-0474cc0540794704ab30615ef80179f4 |
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| Source note | uspto-grants-1988_09 |
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