Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Triphosgene | HCID 94429 | — |
| Reactant | HCID 178501128 | HCID 178501128 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 178501107 | HCID 178501107 | 55.9% |
Reaction Steps
Triphosgene (1.3 mmol, 0.39 g) was added portion wise to a solution of trans-4-{[2-(2-amino-phenyl)-acetylamino]-methyl}-cyclohexanecarboxylic acid methyl ester (2.6 mmol, 0.75 g) in dry CH3CN (20 mL) under argon at 0° C. Then the mixture was heated at 80° C. for 1 h with microwave irradiation. The excess of reagent was quenched by careful addition of H2O (2 mL), the solvent was removed under reduced pressure and the crude was purify by flash chromatography on silica (EtOAc-ETP 10:90 to 50:50) to obtain the titled compound (0.24 g, yield 30%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08865704B2 |
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| Source dataset | uspto-grants-2014_10 |
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| ORD ID | ord-a64b4e0d56894f78bda28f77b4ff2981 |
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| Source note | uspto-grants-2014_10 |
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