HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetone → HCID 66767284, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetone | HCID 180 | — |
| Reactant | Trifluoroacetic acid | HCID 6422 | — |
| Reactant | HCID 66767080 | HCID 66767080 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 66767284 | HCID 66767284 | 86.1% |
Reaction Steps
To a solution of ethyl 5-(2-fluoro-4-nitrophenoxy)-1-(tetrahydro-2H-pyran-2-yl)-1H-indazole-6-carboxylate (15 g, 35 mmol) in DCM (300 mL) is added trifluoroacetic acid (TFA) (30 mL), and stirred at RT overnight. DCM is evaporated. The residue is partitioned between EtOAc (800 mL) and 5% aqueous NaHCO3 (400 mL). The organic layer is washed with saturated aqueous sodium chloride, dried over MgSO4, and concentrated. The residue is purified by silica gel column chromatography eluting with PE:acetone (5:1) to afford the product (10.4 g, 86% yield). MS (m/z): 346.1 (M+H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08030302B2 |
| Source dataset | uspto-grants-2011_10 |
| ORD ID | ord-14aa15675f5a4a6f9544c25e1b9ded09 |
| Source note | uspto-grants-2011_10 |