Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Tetrahydrofuran | HCID 8028 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 1,1'-(9,9-Dimethyl-9H-xanthene-4,5-diyl)bis(1,1-diphenylphosphine) | HCID 636044 | — |
| Reactant | HCID 118251652 | HCID 118251652 | — |
| Catalyst | Molybdenum carbonyl (Mo(CO)6) | HCID 98885 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 118251610 | HCID 118251610 | — |
Reaction Steps
A mixture of compound 64 (0.1 g, 0.231 mmol), molybdenumhexacarbonyl (0.03 g, 0.115 mmol), Hermann's catalyst (0.022 g, 0.023 mmol), Xantphos (0.027 g, 0.0426 mmol), triethylamine (0.643 mL, 0.462 mmol) in a mixture of tetrahydrofuran (3 mL) and methanol (0.9 mL) was heated at 150° C. under microwave conditions for 10 minutes. Then, the reaction was quenched by adding water and diluted with ethyl acetate. The organic layer was separated, washed with Brine, dried (MgSO4), filtered and the solvent was evaporated. Then, the residue was purified by chromatography column on a 20 g SPE cartridge to give the title compound as a colorless solid. (0.043 g, 45%)
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09365569B2 |
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| Source dataset | uspto-grants-2016_06 |
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| ORD ID | ord-a79c1e0a01414b9f9dd6ddaf50121748 |
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| Source note | uspto-grants-2016_06 |
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