HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 86638577, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | (4-Amino-3-fluorophenyl)(4-(4-(1,1,1,3,3,3-hexafluoro-2-hydroxypropan-2-yl)benzyl)piperazin-1-yl)methanone | HCID 86638550 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 86638577 | HCID 86638577 | 29.5% |
Reaction Steps
Borane tetrahydrofuran complex (13.05 mmol, 1.26 mL, 1.121 g) was added to a solution of (4-amino-3-fluorophenyl)(4-(4-(1,1,1,3,3,3-hexafluoro-2-hydroxypropan-2-yl)benzyl)piperazin-1-yl)methanone (1.043 mmol, 0.5 g) in tetrahydrofuran (8 mL) under nitrogen and the reaction heated to reflux for 5.5 hours. 5M Hydrochloric acid (10 mL) was added and the reaction was heated to reflux for 30 minutes, and then was cooled to ambient temperature. The product was extracted into dichloromethane (50 mL), washed with water (3×50 mL), dried over magnesium sulphate and concentrated under reduced pressure. The residue was purified by preparative HPLC affording the title compound (0.143 g). MS (ESI) m/z 466.0 [M+H]+
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08357679B2 |
| Source dataset | uspto-grants-2013_01 |
| ORD ID | ord-8026d62bc5c64e45ae0f40d661f98936 |
| Source note | uspto-grants-2013_01 |