HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethyl 2-(cyclopentanecarboxamido)-3-mercaptopropanoate → Ethyl 2-cyclopentyl-4,5-dihydrothiazole-4-carboxylate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethyl 2-(cyclopentanecarboxamido)-3-mercaptopropanoate | HCID 57989260 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | Ethyl 2-cyclopentyl-4,5-dihydrothiazole-4-carboxylate | HCID 57989100 | — |
Reaction Steps
Tosic acid monohydrate (0.78 g) was added to a solution of ethyl 2-(cyclopentanecarboxamido)-3-mercaptopropanoate [Carboxylic Acid 2, step a] (5 g) in toluene (40 mL). The resulting mixture was heated at reflux under Dean and Stark conditions for 6 h. The reaction was allowed to cool, then the toluene solution was washed with saturated sodium bicarbonate solution (20 mL) and the solvent evaporated. The residue was azeotroped with toluene. The resulting white solid was purified by silica gel chromatography eluting with 9:1 isohexane:ethyl acetate. The fractions containing the product were combined and evaporated to give the subtitled compound as a clear oil. Yield 3.2 g.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08476265B2 |
| Source dataset | uspto-grants-2013_07 |
| ORD ID | ord-d73df788d1db470dbe46f704e87ec044 |
| Source note | uspto-grants-2013_07 |