HuagongsheHuagongshe Chemistry Print Report · For research reference only
Trifluoroacetic acid → HCID 69150976, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Trifluoroacetic acid | HCID 6422 | — |
| Reactant | HCID 69153176 | HCID 69153176 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 69150976 | HCID 69150976 | 53.1% |
Reaction Steps
The title compound was prepared according to the procedure described in Example 3 (Step b) using tert-butyl 3-[N-((1R)-1-[(4-chlorophenyl)methyl]-2-(4-[2-(hydroxyethyl)phenyl]-piperidyl]-2-oxoethyl)carbamoyl]-(3S)-1,2,3,4-tetrahydroisoquinoline-2-carboxylate (Step f) (323 mg, 0.5 mmol) and 50% TFA in CH2Cl2 (20 mL). Purification by reverse phase preparative HPLC (Phenomenex; 5 μm 250×21.2 mm, 5% to 95% CH3CN (0.1% TFA) in H2O (0.1% TFA) over 30 min, then 100% CH3CN (0.1% TFA) for 2 min] provided the title compound (TFA salt) as a white solid (145 mg). MS (ESI, pos. ion) m/z: 546 (M+1); (ESI, neg. ion) m/z: 544 (M−1). Calc'd for C32H36ClN3O3: 545.24.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06977264B2 |
| Source dataset | uspto-grants-2005_12 |
| ORD ID | ord-cbdb255792664524b57aa82374180b05 |
| Source note | uspto-grants-2005_12 |