HuagongsheHuagongshe Chemistry Print Report · For research reference only
Lawesson's reagent → Ethyl 5-amino-2-phenyl-1,3-thiazole-4-carboxylate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Lawesson's reagent | HCID 87949 | — |
| Reactant | HCID 3844040 | HCID 3844040 | — |
| Solvent | Pyridine | HCID 1049 | — |
| Product | Ethyl 5-amino-2-phenyl-1,3-thiazole-4-carboxylate | HCID 13514498 | 40.3% |
Reaction Steps
To a stirred solution of compound ethyl 2-benzamido-2-cyanoacetate (0.46 g, 2 mmol) in pyridine (20 mL) was added Lawesson's reagent (0.81 g, 2 mmol). The reaction mixture was heated at reflux for 15 hr. It was then concentrated and diluted with EtOAc (40 mL). The diluted mixture was washed with water (3×20 mL), brine (10 mL), dried over Na2SO4, filtered, and concentrated in vacuo. The residue was purified by silica gel column chromatography (10:1 PE/EtOAc) to afford ethyl 5-amino-2-phenylthiazole-4-carboxylate (0.2 g, 40%) as yellow solid: 1H-NMR (CDCl3, 500 MHz) δ (ppm): 7.80 (d, J=6.5 Hz, 1H), 7.36-7.41 (m, 3H), 4.43 (q, J=7.0 Hz, 2H), 1.44 (t, J=7.0 Hz, 3H); MS (ESI) m/z: 249 [M+H+].
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08436001B2 |
| Source dataset | uspto-grants-2013_05 |
| ORD ID | ord-65367220608449919a3c584ee2547e91 |
| Source note | uspto-grants-2013_05 |