HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sulfuric Acid → HCID 178421603, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sulfuric Acid | HCID 1118 | — |
| Reactant | Potassium Fluoride | HCID 522689 | — |
| Reactant | HCID 178421607 | HCID 178421607 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 178421603 | HCID 178421603 | 66.1% |
Reaction Steps
To a solution of 6-methyl-3-(3-phenylpropyl)-6-{3-[5-(trimethylsilyl)-1H-1,2,3-triazol-4-yl]phenyl}-3-azabicyclo[3.1.0]hexan-2-one (Preparation 38, 58.0 mg, 0.13 mmol) in ethanol (2 ml) was added potassium fluoride (8.3 mg, 0.14 mmol) and a drop of concentrated sulphuric acid. The mixture was heated at reflux for 4 hours and then stirred at room temperature for 16 hours. The solvent was removed in vacuo and the crude residue was absorbed onto silica. This material was then purified by silica column chromatography eluting first with hexane:ethyl acetate (1:1) and then increasing gradually to neat ethyl acetate. The desired title compound (32 mg, 66%) was isolated as a colourless oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07049444B2 |
| Source dataset | uspto-grants-2006_05 |
| ORD ID | ord-9134e99415574c06936d8d8cc938d092 |
| Source note | uspto-grants-2006_05 |