Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | 1-Butanol | HCID 263 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | HCID 86694728 | HCID 86694728 | — |
| Reactant | HCID 178478345 | HCID 178478345 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 178461872 | HCID 178461872 | — |
Reaction Steps
A 5 mL microwave tube was charged with 126 (208.2 mg, 0.85 mmol), 53 (100 mg, 0.42 mmol) and n-BuOH (1.2 mL) then DIPEA (0.371 mL) was added, the tube sealed and heated to 140° C. for 18 h in an oil bath. The reaction cooled and diluted with EtOAc (50 mL). Water (25 mL) and some MeOH (1 mL) were added and the phases were separated. The organic layer was washed with brine (25 mL), dried (Na2SO4), filtered and concentrated. The residue was purified by HPLC and SFC to afford 34.4 mg (22%) of I-5 as a white solid: SFC RT=0.72 min.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08637537B2 |
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| Source dataset | uspto-grants-2014_01 |
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| ORD ID | ord-46d0bb890f4a419f95b06bd43643b7ce |
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| Source note | uspto-grants-2014_01 |
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