Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Dimethylformamide | HCID 6228 | — |
| Reactant | Lithium Chloride | HCID 433294 | — |
| Reactant | HCID 69560666 | HCID 69560666 | — |
| Catalyst | HCID 178418476 | HCID 178418476 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 69561981 | HCID 69561981 | — |
Reaction Steps
A solution of Example 13I (70 mg, 0.23 mmol), dichlorobis(triphenylphosphine)palladium (II) (7.0 mg, 0.01 mmol), and LiCl (31 mg, 0.73 mmol) in DMF (1.7 mL) was treated dropwise with a solution of Example 13E (120 mg, 0.26 mmol) in DMF (0.2 mL). The mixture was heated to 80° C., stirred for 1.75 hours, cooled to room temperature, diluted with ethyl acetate, washed with H2O and brine, dried (MgSO4), filtered, and concentrated. The concentrate was purified by flash column chromatography on silica gel with 30% ethyl acetate/hexanes to provide the desired product.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06495562B1 |
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| Source dataset | uspto-grants-2002_12 |
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| ORD ID | ord-6699ac0572de40a29d93531938b80132 |
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| Source note | uspto-grants-2002_12 |
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