Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Dimethylformamide | HCID 6228 | — |
| Reactant | O-Phenylenediamine | HCID 7243 | — |
| Reactant | 1-Hydroxybenzotriazole | HCID 75771 | — |
| Reactant | HCID 68418414 | HCID 68418414 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 68415976 | HCID 68415976 | 8% |
Reaction Steps
To a suspension of 4-((4-(3-(cyclopropylamino)-1-(4-fluorophenyl)-3-oxoprop-1-en-2-yl)phenylamino)methyl)benzoic acid (0.215 g, 0.5 mmol) in DMF (3 mL) EDCl (0.23 g, 1.1 mmol), HOBt (0.08 g, 0.55 mmol), o-phenylene diamine (0.086 g, 0.7 mmol), were added followed by TEA (0.2 mL, 1.5 mmol). The reaction mixture was stirred for 4 hours after which the mixture was added to cold water (100 mL) and kept at 0° C. for 1 hour. The pale yellow solid formed was filtered and washed with ethyl acetate (15 mL) dried under vacuum to afford the title compound (0.020 g, 8% yield). 1H NMR (DMSO-d6) δ (ppm): 0.46-0.47 (2H, m, —CH2), 0.60-0.62 (2H, m, —CH2), 2.70-2.71 (1H, m, —CH), 4.36-4.37 (2H, d, —CH2), 4.88 (2H, s, —NH2), 6.55-6.61 (4H, m, Ar—H and —NH), 6.76-6.82 (3H, m, Ar—H), 6.93-6.94 (1H, t, Ar—H), 6.98-7.04 (3H, m, Ar—H), 7.06-7.17 (3H, m, Ar—H), 7.48-7.50 (3H, m, Ar—H and ═CH), 7.93-7.95 (2H, d, Ar—H and —NH), 9.61 (1H, s, —NH), MS m/z: 521.1 (M++1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08450525B2 |
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| Source dataset | uspto-grants-2013_05 |
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| ORD ID | ord-e58cd596b26946a5a742735f62cec382 |
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| Source note | uspto-grants-2013_05 |
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