HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 21949856, compound → HCID 21949766, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 21949856 | HCID 21949856 | — |
| Catalyst | Iron chloride (FeCl3) | HCID 24380 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 21949766 | HCID 21949766 | 75.8% |
Reaction Steps
Iron(III)chloride (9.30 g, 57.5 mmol) was added to a solution of the pyrazole from Example 147 (2.10 g, 5.75 mmol) in dichloromethane (90 ml) under nitrogen at room temperature. After stirring for 20 minutes the mixture was diluted with dichloromethane (50 ml), washed with water (100 ml) then saturated aqueous sodium ethylenediaminetetraacetate solution (70 ml), dried over magnesium sulphate and concentrated under reduced pressure. The residue was purified by flash chromatography on silica gel eluting with dichloromethane:methanol (98:2 changing to 95:5, by volume) to provide the title compound (1.2 g) as a brown oil which solidified on standing.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08063044B2 |
| Source dataset | uspto-grants-2011_11 |
| ORD ID | ord-51c11ff1459a48c38555dc6e1a400eb9 |
| Source note | uspto-grants-2011_11 |