HuagongsheHuagongshe Chemistry Print Report · For research reference only
Trifluoroacetic acid → HCID 56598941, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Trifluoroacetic acid | HCID 6422 | — |
| Reactant | HCID 68078480 | HCID 68078480 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 56598941 | HCID 56598941 | — |
Reaction Steps
To a solution of 1,1-dimethylethyl {2-[6-cyclopropyl-4-({[(4,6-dimethyl-2-oxo-1,2-dihydro-3-pyridinyl)methyl]amino}carbonyl)-1H-pyrazolo[3,4-b]pyridin-1-yl]ethyl}carbamate (260 mg, 0.541 mmol) in DCM (15 mL) was added trifluoroacetic acid (3 ml, 38.9 mmol) and the mixture stirred at room temperature for 2 h. The contents were concentrated in vacuo and the crude residue purified by reverse phase HPLC. (mobile phase: 10 to 70% ACN in H2O, 0.1% NH4OH). The final product was collected as 0.170 g (89%). LCMS E-S (M+H)=353.3 1H NMR (400 MHz, DMSO-d6) δ ppm 1.07 (d, J=6.32 Hz, 4H), 2.13 (s, 3H), 2.21 (s, 4H), 3.00 (t, J=6.19 Hz, 2H), 4.29-4.47 (m, 4H), 5.90 (s, 1H) 7.43 (s, 1H), 8.22 (s, 1H), 8.75 (t, 1H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08637509B2 |
| Source dataset | uspto-grants-2014_01 |
| ORD ID | ord-81f7d321094c473db47ba9570934ea50 |
| Source note | uspto-grants-2014_01 |