HuagongsheHuagongshe Chemistry Print Report · For research reference only
Trifluoroacetic acid → Trifluoroacetic acid
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Trifluoroacetic acid | HCID 6422 | — |
| Reactant | HCID 67539780 | HCID 67539780 | — |
| Catalyst | Adams' catalyst | HCID 345198 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | Trifluoroacetic acid | HCID 6422 | 27% |
| Product | HCID 67539197 | HCID 67539197 | — |
Reaction Steps
A solution of 4-(7-Methyl-pyrido[2,3-d]pyrimidin-4-yl)-piperazine-1-carboxylic acid tert-butyl ester (1.2 g, 3.64 mmol), PtO2 (42 mg, 0.18 mmol) in MeOH (40 mL) and TFA (2 mL) was stirred under H2 (1 atm) at room temperature for 4 hours. The catalyst was filtered and the solvent was removed. The residue was subject to column chromatography, eluted by DCM/MeOH (20:1) to give 4-(7-Methyl-5,6,7,8-tetrahydro-pyrido[2,3-d]pyrimidin-4-yl)-piperazine-1-carboxylic acid tert-butyl ester as TFA salt (0.43 g, 27%). 1H NMR (CDCl3, 400 MHz) δ 9.75 (s, 1H), 7.97 (s, 1H), 3.60 (m, 10H), 2.60 (m, 2H), 2.00 (m, 1H), 1.48 (s, 9H), 1.35 (d, J=6.4 Hz, 3H). MS (APCI+) [M+H]+334.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08680114B2 |
| Source dataset | uspto-grants-2014_03 |
| ORD ID | ord-62ad1bc0b75c4565b5ca38be812057bb |
| Source note | uspto-grants-2014_03 |