Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Sodium Carbonate | HCID 10340 | — |
| Reactant | 4-Chloro-2-(1,1-dimethylethyl)-5-mercapto-3(2H)-pyridazinone | HCID 13469242 | — |
| Reactant | HCID 19863326 | HCID 19863326 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 14623063 | HCID 14623063 | 94.1% |
Reaction Steps
In 50 ml of N,N-dimethylformamide were dissolved 6.6 g of 2-t-butyl-4-chloro-5-mercapto-3(2H)-pyridazinone and 10 g of 2-(2',6'-dimethyl-4'-benzoylphenoxy)ethyl bromide, and thereto was added 5 g of anhydrous sodium carbonate. The solution was stirred at room temperature for seventeen hours. The resulting solution was poured into water and extracted with diethyl ether. The organic layer was dried over anhydrous sodium sulfate and freed of solvent by distillation under reduced pressure to give a crude product. The crude product thus obtained was purified by means of column chromatography (on silica gel, eluting with benzene) and crystallization (from 50 ml of n-hexanediethyl ether (4:1)) to give 13.3 g of the intended compound. m.p. 94.6°~96.2° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US04906627 |
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| Source dataset | uspto-grants-1990_03 |
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| ORD ID | ord-427ccc58dcce440bb2ee518b45a66405 |
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| Source note | uspto-grants-1990_03 |
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