HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → HCID 86729619, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Trifluoroacetic acid | HCID 6422 | — |
| Reactant | HCID 86729620 | HCID 86729620 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 86729619 | HCID 86729619 | — |
Reaction Steps
To a solution of (S)-tert-butyl 3-(4-(2-acrylamidophenylamino)-5-(trifluoromethyl)pyrimidin-2-ylamino)piperidine-1-carboxylate (3 g) in DCM (30 ml) was added trifluoroacetic acid (5 ml) at 0° C. for 10 min and stirred at rt for 2 h. TLC showed completion of starting material. (TLC system: 15% methanol in dichloromethane, Rf=0.2). The reaction mixture was concentrated, and the crude was co-distilled with DCM (3×20 mL) and washed with diethyl ether (2×10 mL) to obtain (S)—N-(2-(2-(piperidin-3-ylamino)-5-(trifluoromethyl) pyrimidin-4-ylamino)phenyl)acrylamide as an off white solid. (3 g, 97%). MS: m/z=407.1 (ES+, M+H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09145387B2 |
| Source dataset | uspto-grants-2015_09 |
| ORD ID | ord-e1dcf8d6ee004f888d228793055b8d1e |
| Source note | uspto-grants-2015_09 |