HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethyl chloroformate → HCID 58677551, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethyl chloroformate | HCID 10928 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | (5-Amino-2-methyl-phenyl)-[2-chloro-4-(2,4-difluoro-phenylamino)-phenyl]-methanone | HCID 11538012 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 58677551 | HCID 58677551 | — |
Reaction Steps
Compound 494 (0.039 g, 0.1 mmol) was suspended in dry CH2Cl2 (1 mL) under an argon atmosphere. K2CO3 (0.029 g, 0.21 mmol) was added followed by ethyl chloroformate (0.02 mL, 0.021 mmol). The suspension was stirred for 48 h at room temperature. Work up as described in the preparation of compound 277. The crude product was purified by flash chromatography using EtOAc/petroleum ether (40-60) 1:2 as the eluent. This afforded the title compound as oil. 13C NMR (CDCl3) δ 196.0, 159.1 (dd), 155.6 (dd), 153.7, 147.9, 139.5, 135.6, 135.1, 133.6, 132.6, 131.9, 129.1, 124.4 (dd), 124.3 (dd), 121.3, 119.8, 116.2, 112.7, 111.6 (dd), 104.9 (dd), 61.3, 19.7, 14.5
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07977387B2 |
| Source dataset | uspto-grants-2011_07 |
| ORD ID | ord-968994ffee804ce9a5f5ecffc621c945 |
| Source note | uspto-grants-2011_07 |