Participants
| Role | Name | HCID | Charge |
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| Reactant | Methylamine | HCID 6329 | — |
| Reactant | HCID 23448012 | HCID 23448012 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 23448019 | HCID 23448019 | — |
Reaction Steps
To a solution of methylamine (1 ml, 40% in methanol) in dichloromethane (1 ml) was added 11-chloro-6-(2-dimethylamino-ethylamino)-3-methoxy-5,10-diaza-benzo[c]fluoren-7-one (Example 27e) (5.7 mg) and the mixture was stirred at 50° C. for 2 days in a sealed tube. The solution was diluted with dichloromethane and washed with saturated ammonium chloride aqueous solution and dried over anhydrous sodium sulfate and evaporated to dryness. The residue was purified by silica gel thin layer chromatography developed by dichloromethane-methanol=4:1. The desired product was obtained as a dark red powder (1.8 mg). ESI−MS: m/z 378 (MH+); 1H-NMR (CDCl3): δ2.44 (6H, s), 2.77 (2H, t, J=6.3 Hz), 3.14 (3H, d, J=4.9 Hz), 3.82 (2H, q-like, J=6.3 Hz), 3.96 (3H, s), 4.85 (1H, brq, J=ca 5 Hz), 6.89-6.95 (2H, m), 7.04 (1H, d, J=2.6 Hz), 7.30 (1H, brt, J=ca 6 Hz), 8.34 (1H, d, J=9.2 Hz), 8.41 (1H, d, J=4.3 Hz).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06680326B2 |
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| Source dataset | uspto-grants-2004_01 |
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| ORD ID | ord-dcb269ef02824c0582411bebdfbe0b87 |
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| Source note | uspto-grants-2004_01 |
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