Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Lithium Chloride | HCID 433294 | — |
| Reactant | Tris(furan-2-yl)phosphane | HCID 521585 | — |
| Reactant | HCID 18789311 | HCID 18789311 | — |
| Reactant | Tri(butyl)vinyltin | HCID 53438229 | — |
| Solvent | N-methyl-2-pyrrolidone | HCID 13387 | — |
| Solvent | Ethyl acetate hexane | HCID 21226206 | — |
| Product | HCID 18789323 | HCID 18789323 | — |
Reaction Steps
5-(4-Bromophenyl)-3-(2-indanyl)carbonylaminopyrazole (106.5 mg), tributylvinyltin (0.25 ml), a tris(dibenzylideneacetone)dipalladium chloroform complex (17.1 mg), tri-2-furylphosphine (34.4 mg) and lithium chloride (34.0 mg) were dissolved in N-methylpyrrolidone (2 ml) with heating, and the resultant mixture was heated at 80° C. overnight. After allowing to cool, the reaction solution was diluted with ethyl acetate-hexane (1:1, 100 ml), washed with saturated aqueous potassium fluoride solution (100 ml×2) and then dried over anhydrous magnesium sulfate. The solvent was distilled away under a reduced pressure. The resultant residue was purified by column chromatography on silica gel (ethyl acetate:hexane=1:1) and then crystallized from chloroform to obtain the title compound (70.2 mg) as white crystals (melting point: 193-195° C.).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06057335 |
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| Source dataset | uspto-grants-2000_05 |
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| ORD ID | ord-d41a0a12af6f4a5389a496901cd47345 |
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| Source note | uspto-grants-2000_05 |
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