Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Isopropylamine | HCID 6363 | — |
| Reactant | HCID 11984297 | HCID 11984297 | — |
| Product | HCID 59645231 | HCID 59645231 | — |
Reaction Steps
In an oven-dried high pressure bomb reactor apparatus was placed dry toluene (30 mL) and nitrogen was bubbled through the solution. Methyl 2-{[(tert-butoxycarbonyl)amino]methyl}-5-fluorobenzoate (4.0 g, 14.1 mmol, prepared as described in Example 3C, Step 4) and isopropylamine (12.0 mL, 0.14 mol) were added to the vessel. The bomb was sealed and heated to 70° C. overnight. The vessel was cooled and the reaction was concentrated to dryness in vacuo. The residue was purifed by flash column chromatography (ISCO column, 120 g silica) running a 0-30% acetone/hexane gradient over 30 minutes. The product fractions were concentrated to give the title compound as a white solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07323460B2 |
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| Source dataset | uspto-grants-2008_01 |
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| ORD ID | ord-b0ea0cc5a8cc44b594f18606f6ab3d3b |
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| Source note | uspto-grants-2008_01 |
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