Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Methylamine | HCID 6329 | — |
| Reactant | 1,1'-Carbonyldiimidazole | HCID 68263 | — |
| Reactant | HCID 67125458 | HCID 67125458 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 67125394 | HCID 67125394 | — |
Reaction Steps
To 100 mg (0.31 mmol) (S)-1-{4-[1-(4-ethoxy-phenyl)-piperidin-4-yl]-phenyl}-ethylamine (XIII.1) in 2 mL DMF, 87 μL (0.62 mmol) TEA and 52 mg (0.32 mmol) CDI are added at 0° C. and the mixture is stirred for 30 min at 0° C. Subsequently 48 mg (1.54 mmol) methylamine are added and stirring is continued for 1 h at 50° C. The mixture is filtered through basic aluminum oxide and concentrated in vacuo. The residue is purified using reversed phase column chromatography (water+0.15% NH4OH; acetone) and the corresponding fractions are concentrated to yield the desired product.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09006450B2 |
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| Source dataset | uspto-grants-2015_04 |
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| ORD ID | ord-0c3c5781e05d4500b6c45048585df158 |
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| Source note | uspto-grants-2015_04 |
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