HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Carbonate → HCID 58677613, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | Allyl chloroformate | HCID 18052 | — |
| Reactant | (5-Amino-2-methyl-phenyl)-[2-chloro-4-(2,4-difluoro-phenylamino)-phenyl]-methanone | HCID 11538012 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 58677613 | HCID 58677613 | — |
Reaction Steps
Compound 494 (0.06 g, 0.16 mmol) was suspended in dry CH2Cl2 (1.5 mL) under an argon atmosphere in a screw cap vessel. K2CO3 (0.044 g, 0.32 mmol) was added followed by allyl chloroformate (0.034 mL, 0.032 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 a gradient of EtOAc/petroleum ether (40-60) 5:95→30:70 as the eluent. This afforded the title compound as yellow oil. 13C NMR (CDCl3) δ 195.8, 159.1 (dd), 155.5 (dd), 153.2, 147.7, 139.6, 135.4, 135.2, 133.6, 132.9, 132.3, 132.0, 129.3, 124.4 (dd), 124.2 (dd), 121.3, 119.7, 118.3, 116.3, 112.8, 111.6 (dd), 105.0 (dd), 65.9, 19.7
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07977387B2 |
| Source dataset | uspto-grants-2011_07 |
| ORD ID | ord-383e0d9b825847459877249500f60791 |
| Source note | uspto-grants-2011_07 |