HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → HCID 46244492, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Trifluoroacetic acid | HCID 6422 | — |
| Reactant | HCID 86761740 | HCID 86761740 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 46244492 | HCID 46244492 | 53.1% |
Reaction Steps
5-(2-Chloro-5-fluoro-benzyloxy)-3-{4-(4-methyl-piperazin-1-yl)-2-[(tetrahydro-pyran-4-yl)-(2,2,2-trifluoro-acetyl)-amino]-benzoylamino}-indazole-1-carboxylic acid tert-butyl ester (100 mg, 0.1269 mmol) in DCM (1.3 mL) was treated at room temperature with TFA (0.195 mL, 2.538 mmol). After 2 hours the volatiles were evaporated and the residue was treated with MeOH (3 mL) and TEA (0.357 mL, 2.538 mmol) and refluxed for three hours. After evaporation of the volatile components the crude was diluted with DCM (25 mL), washed with water, aqueous NaHCO3, water and finally brine, dried over sodium sulfate, evaporated and purified by flash chromatography over silica gel (eluent: DCM:7N NH3 in MeOH 93:7) to give 40 mg of title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08354399B2 |
| Source dataset | uspto-grants-2013_01 |
| ORD ID | ord-b15fe902e04045dc8c52ed6409f68928 |
| Source note | uspto-grants-2013_01 |