Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Dimethylamine, hydrochloride | HCID 10473 | — |
| Reactant | HCID 22981229 | HCID 22981229 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 22981211 | HCID 22981211 | 103% |
Reaction Steps
A mixture of the compound (1.0 g) obtained in Example 263, dimethylamine hydrochloride (485 mg), triethylamine (0.8 ml) and dimethylformamide (10 ml) was heated at 80° C. for 5.5 h. The reaction mixture was distilled under reduced pressure and water and 2 N HCl were added to the residue; after extraction with ethyl acetate, the organic layer was washed with a saturated aqueous sodium chloride solution, dried with anhydrous magnesium sulfate and concentrated under reduced pressure. The resulting residue was purified by silica gel column chromatography (eluent, n-hexane:ethyl acetate=3:1) to give 1.1 g of the titled compound quantitatively.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06534546B1 |
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| Source dataset | uspto-grants-2003_03 |
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| ORD ID | ord-2417f77fbdf84c2db5fbdd0f0ca964a6 |
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| Source note | uspto-grants-2003_03 |
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