HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 59443072, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | 1,4-Dioxane | HCID 31275 | — |
| Reactant | HCID 59443032 | HCID 59443032 | — |
| Product | HCID 59443072 | HCID 59443072 | — |
Reaction Steps
6N Hydrochloric acid (15 mL) was added to a solution of tert-butyl [3-cyano-4-(4-fluorophenyl)-2,2-dimethyl-2H-chromen-7-yl]carbamate (a compound obtained in Reference Example 8(3); 150 mg) in dioxane (5 mL) and the mixture was heated under reflux for 90 hours. The reaction solution was concentrated in vacuo, the resulted residue was diluted with ethyl acetate and washed with a saturated solution of sodium bicarbonate and brine. The organic layer was filtered through a column of porous diatomite (Chem Elut) and the filtrate was concentrated in vacuo. The resultant residue was purified by column chromatography on silica gel (Solvent: chloroform/methanol=100/0 to 95/5) to give the titled compound (26 mg) as a yellow powder.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08258131B2 |
| Source dataset | uspto-grants-2012_09 |
| ORD ID | ord-2d345a085f1b466abbdfec68b04e5fd1 |
| Source note | uspto-grants-2012_09 |