HuagongsheHuagongshe Chemistry Print Report · For research reference only
Trifluoroacetic acid → HCID 66846592, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Trifluoroacetic acid | HCID 6422 | — |
| Reactant | HCID 66846317 | HCID 66846317 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 66846592 | HCID 66846592 | 55.4% |
Reaction Steps
The product of Example 20F (0.8 g, 2.22 mmol) was treated with TFA (5 mL) in CH2Cl2 (10 mL) at ambient temperature for 1 h. The mixture was then concentrated under reduced pressure and the residue was purified by column chromatography (SiO2, 90:9:1 CH2Cl2:MeOH:NH4OH) to give the title compound (0.32 g, 1.23 mmol, 55% yield). 1H NMR (MeOH-d4, 300 MHz) δ 1.42, 1.47 (s, 3H, rotamers), 1.63-1.75 (m, 1H), 1.98-2.13 (m, 1H), 2.37-2.52 (m, 1H), 2.62-2.76 (m, 2H), 3.00-3.12 (m, 1H), 3.26, 3.47 (d, J=12.6 Hz, 1H, rotamers), 3.53-3.62 (m, 2H), 5.08, 5.13 (s, 2H, rotamers), 7.25-7.42 (m, 5H); MS (DCl/NH3) m/z 261 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07872010B2 |
| Source dataset | uspto-grants-2011_01 |
| ORD ID | ord-b24974f40c1d4e44aa827cf040744059 |
| Source note | uspto-grants-2011_01 |