Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Sodium Carbonate | HCID 10340 | — |
| Reactant | 1,1'-Carbonyldiimidazole | HCID 68263 | — |
| Reactant | HCID 67166426 | HCID 67166426 | — |
| Reactant | HCID 67167837 | HCID 67167837 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 67166898 | HCID 67166898 | 57% |
Reaction Steps
Under an inert atmosphere, 0.18 g of N,N-carbonyldiimidazole is added to a suspension of 0.4 g (1.1 mmol) of the compound obtained from step 2.5 in DMF (5 ml). The reaction mixture is stirred at room temperature for 1 hour 30 minutes, 0.225 g (1.2 mmol) of the compound obtained from step 2.2 dissolved in DMF (1 ml), and stirred beforehand in the presence of 0.13 g (1.3 mmol) of sodium carbonate, is then added and the mixture is heated at 80° C. for 2 hours. The DMF is removed by evaporation under reduced pressure, and the residue is then purified by flash chromatography on silica gel (eluent: dichloromethane/methanol/1% NH4OH), with a gradient of 0% to 5% methanol. 0.3 g of product is obtained, in the form of a white powder. Yield: 57%. MH+: 521.3
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US08436011B2 |
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| Source dataset | uspto-grants-2013_05 |
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| ORD ID | ord-edc7728f9aab473daa401fbf80b63c41 |
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| Source note | uspto-grants-2013_05 |
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