Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Phenyl isocyanate | HCID 7672 | — |
| Reactant | (5-Amino-2-methyl-phenyl)-[2-chloro-4-(2,4-difluoro-phenylamino)-phenyl]-methanone | HCID 11538012 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 58677581 | HCID 58677581 | — |
Reaction Steps
Compound 494 (0.03 g, 0.08 mmol) was dissolved in 1,4-dioxan (0.5 mL) and phenyl isocyanate (0.013 mL, 0.12 mmol) was added. The solution was stirred at 50° C. for 18 h. Work up as described in the preparation of compound 259. The crude product was purified by flash chromatography using a gradient of EtOAc/petroleum ether (40-60) 15:85→60:40 as the eluent. This afforded the title compound as an amorphous compound. 13C NMR (DMSO-d6) δ 195.1, 158.7 (dd), 155.7 (dd), 152.3, 148.9, 139.3, 139.1, 137.2, 133.4, 131.5, 129.6, 128.7, 127.0, 126.2 (dd), 124.2 (dd), 121.8, 120.3, 118.4, 118.2, 118.1, 114.8, 111.9 (dd), 111.8, 105.0 (dd), 19.0
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US07977387B2 |
|---|
| Source dataset | uspto-grants-2011_07 |
|---|
| ORD ID | ord-098bf3663cce4991ba8476924d917a0d |
|---|
| Source note | uspto-grants-2011_07 |
|---|
