HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 24986539, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Methanol | HCID 887 | — |
| Reactant | HCID 66736072 | HCID 66736072 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 24986539 | HCID 24986539 | — |
Reaction Steps
The crude N-[5-(3,5-difluoro-benzenesulfonyl)-1-trityl-1H-indazol-3-yl]-4-(4-pyrrolidin-1-yl-piperidine-1-carbonyl)-benzamide was treated with 15 mL of 1,4-dioxane and with 4M hydrochloric acid in 1,4-dioxane (4 mL). The mixture was stirred at room temperature for 2 days then treated with methanol (15 mL) and stirred for additional 3 hours. The solvents were removed under reduced pressure and the residue taken up with ethyl acetate, washed with 10% aqueous ammonium hydroxide, dried over sodium sulfate and evaporated to dryness. The crude was purified by flash chromatography over silica gel eluting with dichloromethane/methanol/7N NH3 in methanol 100:7:1 affording 185 mg of the title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08114865B2 |
| Source dataset | uspto-grants-2012_02 |
| ORD ID | ord-627b2b357f1c49a1af7207ea574b2a98 |
| Source note | uspto-grants-2012_02 |