Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Tert-butyl 3-(2-aminoacetamido)azetidine-1-carboxylate | HCID 18699815 | — |
| Reactant | 1-Chloro-7-(trifluoromethyl)phthalazine | HCID 58562576 | — |
| Solvent | Diglyme | HCID 8150 | — |
| Product | HCID 68004015 | HCID 68004015 | — |
Reaction Steps
Into a 50 mL round-bottom flask, was placed a solution of 1-chloro-7-(trifluoromethyl)phthalazine (prepared as described in the previous step, 1.5 g, 6.47 mmol, 1.00 equiv) in 2-methoxyethyl ether (10 mL), tert-butyl 3-(2-aminoacetamido)azetidine-1-carboxylate (prepared as described in Example 1, Step E) (1.5 g, 6.55 mmol, 1.22 equiv) and triethylamine (1.95 g, 19.31 mmol, 2.99 equiv). The reaction mixture was stirred overnight at 100° C. in an oil bath. The reaction progress was monitored by LCMS. The resulting mixture was concentrated under vacuum. The residue was purified by chromatography over a silica gel column with CH3CN:H2O (3:1). The title compound was obtained as a white solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08518969B2 |
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| Source dataset | uspto-grants-2013_08 |
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| ORD ID | ord-3ccc744dd60f459e994394eb81cb4b79 |
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| Source note | uspto-grants-2013_08 |
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