Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Potassium Phosphate, Tribasic | HCID 62657 | — |
| Reactant | HCID 67074075 | HCID 67074075 | — |
| Reactant | HCID 86652694 | HCID 86652694 | — |
| Catalyst | HCID 178418851 | HCID 178418851 | — |
| Solvent | 1,2-Dimethoxyethane | HCID 8071 | — |
| Product | HCID 86652693 | HCID 86652693 | 35% |
Reaction Steps
A mixture of 0.20 g (0.78 mmol) of 4-((S)-3-Methyl-2-oxo-piperazin-1-yl)-butyric acid tert-butyl ester, 0.1 eq. of HCl, 0.53 g (1.56 mmol) of 4-iodo-1,2-bis-trifluoromethyl-benzene (WO2007034282), 0.04 g (0.078 mmol) bis(tri-tert-butylphosphine)palladium(0) and 0.33 g (1.56 mmol) tripotassium phosphate in 2 ml of 1,2-dimethoxyethane was degased and heated at 120° C. for 2 h under microwave irradiation, diluted with dichloromethane, filtered and evaporated. Purification on a SiO2-column (1-propanol in n-heptane 2 to 5%), gave the titled compound in 35% yield as light brown oil. MS: 413.13 (M[-C4H8]H+).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08445674B2 |
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| Source dataset | uspto-grants-2013_05 |
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| ORD ID | ord-3ed51bd2537f4fc99c961292ede3ddc2 |
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| Source note | uspto-grants-2013_05 |
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