HuagongsheHuagongshe Chemistry Print Report · For research reference only
Cyanoacetic acid → HCID 178456264, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Cyanoacetic acid | HCID 9740 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | Benzotriazol-1-yloxy-tris(dimethylamino)phosphonium hexafluorophosphate | HCID 151348 | — |
| Reactant | HCID 178456263 | HCID 178456263 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 178456264 | HCID 178456264 | 61% |
Reaction Steps
To a suspension of Example 48 and 2-cyanoacetic acid (4.01 mg, 0.047 mmol) in DCM (1 mL) was added DIEA (0.035 mL, 0.200 mmol) and BOP (20.87 mg, 0.047 mmol). The mixture was stirred at room temperature for 30 minutes and then concentrated. The crude reaction mixture was purified by reversed-phase preparative HPLC to give the title compound (8.1 mg, 61%) as white solid. HPLC Rt=2.981 min (Chromolith SpeedROD 4.6×50 mm, 10-90% aqueous methanol containing 0.1% TFA, 4 min gradient, monitored at 220 nm), [M+H]=560.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08389527B2 |
| Source dataset | uspto-grants-2013_03 |
| ORD ID | ord-03a24d07bfab4720a55dbccc4ae2101d |
| Source note | uspto-grants-2013_03 |