Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Piperidine | HCID 8082 | — |
| Reactant | HCID 10309275 | HCID 10309275 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | HCID 10151077 | HCID 10151077 | — |
Reaction Steps
To an oven-dried round bottom flask fitted with a rubber septa was added toluene (1 mL), the product of Step D of Example 114 (0.050 g; 0.134 mmol) and piperidine (0.070 mL; 0.670 mmol). The sealed reaction mixture was heated at 100° C. and stirred for 16 hours. The reaction mixture was allowed to cool to room temperature, then it was partitioned between ethyl acetate and saturated NaHCO3 solution. The organic portion was separated and washed with more saturated NaHCO3 solution (2×), brine, dried (Na2SO4), filtered, and concentrated in vacuo. Purification was done by MPLC (silica gel; 0-10% ethyl acetate:hexane) to afford the desired product: m/e=422 (M+1) Rt=5.10 min on LCMS.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07271266B2 |
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| Source dataset | uspto-grants-2007_09 |
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| ORD ID | ord-a0b7fe51f83d4063bf23d6e616e1e28f |
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| Source note | uspto-grants-2007_09 |
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