HuagongsheHuagongshe Chemistry Print Report · For research reference only
Trifluoroacetic acid → HCID 16666254, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Trifluoroacetic acid | HCID 6422 | — |
| Reactant | HCID 90925078 | HCID 90925078 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 16666254 | HCID 16666254 | 64.5% |
Reaction Steps
A mixture of EXAMPLE 88C (0.26 g, 0.6 mmol) in dichloromethane (5 mL) was treated with trifluoroacetic acid (5 mL) and the mixture stirred at ambient temperature for 4 hours. The mixture was concentrated and purified by flash chromatography on silica gel using 0-10% methanol/dichloromethane/0.1% ammonium hydroxide, followed by HPLC on a C18 column using 0-100% acetonitrile/water/0.1% trifluoroacetic acid, to provide the title compound (0.131 g) as the trifluoroacetate salt. 1HNMR (DMSO-D6) δ 9.22 (s, 1H), 8.63 (s, 1H), 8.38 (s, 1H), 8.21 (d, J=8.3 Hz, 2H), 7.94 (s, 1H), 7.55-7.62 (m, 2H), 7.45 (t, J=7.7 Hz, 2H), 3.40 (s, 2H), 2.99-3.07 (m, 2H), 1.99 (s, 2H), 1.78-1.90 (m, 2H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08697736B2 |
| Source dataset | uspto-grants-2014_04 |
| ORD ID | ord-da04355023aa4b3db8372344d6cc586f |
| Source note | uspto-grants-2014_04 |