HuagongsheHuagongshe Chemistry Print Report · For research reference only
4-Methoxybenzenecarbothioamide → 2-(4-Methoxy-phenyl)-6,7-dihydro-4H-thiazolo[5,4-c]pyridine-5-carboxylic acid benzyl ester
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 4-Methoxybenzenecarbothioamide | HCID 736827 | — |
| Reactant | 3-Bromo-4-oxo-piperidine-1-carboxylic acid benzyl ester | HCID 22407002 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | 2-(4-Methoxy-phenyl)-6,7-dihydro-4H-thiazolo[5,4-c]pyridine-5-carboxylic acid benzyl ester | HCID 66653423 | 49% |
Reaction Steps
Compound 502 (2.0 g, 6.5 mmol) was dissolved in ethanol (20 ml). To the solution was added 4-methoxythiobenzamide (503, 1.09 g, 6.5 mmol, 1 eq) and the yellow mixture was refluxed for 17 hrs after which time TLC analysis showed full conversion of 502. The reaction mixture was concentrated in vacuo and the residue was dissolved in EtOAc, washed with 5% Na2SO4 and the organic layer was dried (MgSO4) and subsequently concentrated under reduced pressure. The resulting oil was purified by silica gel chromatography (diethyl ether, Rf 0.3) giving compound 504 in a yield of 49% as a colorless oil. Compounds having a Rb substitute can be prepared by choosing a properly substituted (Rb)-4-methoxythiobenzamide (503).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08796262B2 |
| Source dataset | uspto-grants-2014_08 |
| ORD ID | ord-e2a5788bc90a485f9e905d75bd346c1d |
| Source note | uspto-grants-2014_08 |