HuagongsheHuagongshe Chemistry Print Report · For research reference only
Trifluoroacetic acid → Trifluoroacetic acid
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Trifluoroacetic acid | HCID 6422 | — |
| Reactant | HCID 86633569 | HCID 86633569 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | Trifluoroacetic acid | HCID 6422 | — |
| Product | HCID 57826397 | HCID 57826397 | — |
Reaction Steps
To a solution of 1,1-dimethylethyl[2-({[3-methyl-4-(1-methyl-1H-pyrazol-5-yl)-2-thienyl]carbonyl}amino)-3-phenylpropyl]carbamate (51 mg, 0.11 mmol) in DCM (1 mL) was added TFA (1 mL). The reaction was stirred over 5 h, concentrated and purified by reverse-phase HPLC (C18 column: H2O/CH3CN, 40-10%) to afford the bis-TFA salt of the title compound. (16 mg, 41%): LC-MS (ES) m/z 355 (M+H)+. NMR (d4-MeOD, 400 MHz) δ ppm 7.64 (s, 1H), 7.56 (d, J=1.8 Hz, 1H), 7.36-7.30 (m, 4H), 7.28-7.21 (m, 1H), 6.30 (d, J=2.0 Hz, 1H), 4.58 (m, 1H), 3.69 (s, 3H), 3.27-3.13 (m, 2H), 3.07-2.93 (m, 2H), and 2.13 (s, 3H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08273782B2 |
| Source dataset | uspto-grants-2012_09 |
| ORD ID | ord-880419ce0aa741518990f162602e2baa |
| Source note | uspto-grants-2012_09 |