Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Sodium Iodide | HCID 5238 | — |
| Reactant | Sodium Carbonate | HCID 10340 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | 3-(1-Piperazinyl)-1,2-benzisothiazole | HCID 2772144 | — |
| Reactant | HCID 19872077 | HCID 19872077 | — |
| Solvent | Methyl Isobutyl Ketone | HCID 7909 | — |
| Product | HCID 86743642 | HCID 86743642 | — |
Reaction Steps
To a 100 ml round-bottomed flask equipped with condenser and N2 inlet were added 1.0 g (4.57 mmol) 3-piperazinyl-benzisothiazole, 1.46 g (4.57 mmol) 4-(4-(2-chloroethyl)phenyl)thiazol-2-one hydrobromide, 970 mg (9.13 mmol) sodium carbonate, 600 mg (4.57 mmol) diisopropylethylamine, 2 mg sodium iodide, and 35 ml methylisobutylketone. The reaction was refluxed 24 hours, cooled, and evaporated. The residue was taken up in ethyl acetate, washed with water and brine, dried over sodium sulfate, and evaporated. The residue was chromatographed on silica gel using methylene chloride/ethyl acetate as eluent. The product fractions were dissolved in methylene chloride/ethyl acetate and precipitated with HCl gas. The precipitate was filtered to give a solid, m.p. 190° C., 455 mg (21.9%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US04891375 |
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| Source dataset | uspto-grants-1990_01 |
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| ORD ID | ord-5b9e49387752491e9b1b262ea0aea22f |
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| Source note | uspto-grants-1990_01 |
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