HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Hydroxide → HCID 178477697, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Hydroxide | HCID 14797 | — |
| Reactant | HCID 178477690 | HCID 178477690 | — |
| Solvent | tert-Butanol | HCID 6386 | — |
| Product | HCID 178477697 | HCID 178477697 | 48% |
Reaction Steps
The mixture of 3-[1-(ethylsulfonyl)-4-piperidinyl]-5-(4-fluorophenyl)-1H-indazole-7-carbonitrile (Intermediate 11) (0.102 mmols) and potassium hydroxide (26 mg, 0.51 mmol) in 2-methyl-2-propanol (4 mL) was heated overnight. The reaction mixture was concentrated and purified by using a Gilson semi-preparative HPLC system with a YMC ODS-A (C-18) column 50 mm by 20 mm ID, eluting with 10% B to 70% B in 3.2 min, hold for 1 min where A=H2O (0.1% trifluoroacetic acid) and B=CH3CN (0.1% trifluoroacetic acid) pumped at 25 mL/min to afford the title compound (21 mg, 48% for 2 steps)
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08501780B2 |
| Source dataset | uspto-grants-2013_08 |
| ORD ID | ord-876669da277c4115b615bc4fd291af2d |
| Source note | uspto-grants-2013_08 |