HuagongsheHuagongshe Chemistry Print Report · For research reference only
Trifluoroacetic acid → HCID 131724943, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Trifluoroacetic acid | HCID 6422 | — |
| Reactant | HCID 131724942 | HCID 131724942 | — |
| Product | HCID 131724943 | HCID 131724943 | 51.3% |
Reaction Steps
The reaction was carried out according to Example 12 step 3 using 1,1-dimethylethyl 5-({[3-(5-methylisoxazol-3-yl)[1,2,4]triazolo[3,4-α]phthalazin-6-yl]oxy}methyl)-3′6′-dihydro-2,4′-bipyridine-1′(2′H)-carboxylate (296 mg, 0.55 mmol) and trifluoroacetic acid (5 ml). The crude residue was purified by column chromatography on silica using 7% MeOH/CH2Cl2 containing 1% NH3 to yield the desired phthalazine (124 mg, 51%). 1H NMR (360 MHz, CDCl3) δ 8.81 (1H, s), 8.68 (1H, d, J=7.6 Hz), 8.21 (1H, d, J=8.0 Hz), 8.05-7.90 (2H, m), 7.80 (1H, t, J=8.0 Hz), 7.43 (1H, t, J=8.1 Hz), 6.85 (1H, s), 6.75 (1H, broad s), 5.68 (2H, s), 3.60 (2H, q, J=2.9 Hz), 3.12 (2H, t, J=5.7 Hz), 2.67-2.55 (5H, m). m/z (ES+) 440 (M+H+).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06900209B2 |
| Source dataset | uspto-grants-2005_05 |
| ORD ID | ord-44f9ddfbc217484cbd6423fccce230b7 |
| Source note | uspto-grants-2005_05 |