Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Methylamine | HCID 6329 | — |
| Reactant | HCID 18387453 | HCID 18387453 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 18387456 | HCID 18387456 | — |
Reaction Steps
Compound 13 as prepared in Example 10 (0.045 g, 0.08 mM) and methylamine (40% solution in water; 1 ml) in tetrahydrofuran (4 ml) was heated in a sealed tube with stirring in an 80° C. oil bath for 16 hours. The mixture was cooled to room temperature, evaporated to dryness, diluted with water (30 ml) and extracted with ethyl acetate (2×35 ml). The combined ethyl acetate extracts were dried (MgSO4) and evaporated in vacuo to give a crude mixture. Purification by chromatography (EM silica Gel 60; 10% EtOAc in CH2Cl2) gave the product as a white solid. m/z (MH+)460.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06489321B1 |
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| Source dataset | uspto-grants-2002_12 |
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| ORD ID | ord-d888401127164abbb2a226353867315f |
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| Source note | uspto-grants-2002_12 |
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