Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Triphosgene | HCID 94429 | — |
| Reactant | HCID 178501121 | HCID 178501121 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 178501097 | HCID 178501097 | 263.9% |
Reaction Steps
To a solution of trans-4-{[2-(2-Amino-phenyl)-ethylamino]-methyl}-cyclohexanecarboxylic acid methyl ester (2.99 g, 7.97 mmol) in CH3CN (100 mL) at 0° C. under argon was added portion wise triphosgene (1.53 g, 5.15 mmol) over 30 min. The reaction mixture was stirred at 0° C. for 30 min, warmed to room temperature and stirred additionally for 7 h. Then an excess of TEA was added and a precipitate was formed. Solvent was removed under reduced pressure and the crude product purified by flash chromatography on silica to afford the titled compound (4.3 g, yield 59%).
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-fb37499baefd496d898cc617bfffda8e |
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| Source note | uspto-grants-2014_10 |
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