HuagongsheHuagongshe Chemistry Print Report · For research reference only
Lawesson's reagent → HCID 178501057, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Lawesson's reagent | HCID 87949 | — |
| Reactant | HCID 178501160 | HCID 178501160 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 178501057 | HCID 178501057 | 82.9% |
Reaction Steps
A solution of trans-4-[2-(6-bromopyridin-2-yl)-2-oxoethylcarbamoyl]cyclohexanecarboxylic acid methyl ester (7.38 g, 19.3 mmol) obtained in Step 2 and a Lawesson reagent (8.20 g, 20.3 mmol) in tetrahydrofuran (120 ml) was heated at reflux for 2 hours in an Ar stream. After the reaction solution was concentrated, a saturated aqueous sodium bicarbonate was added and extracted with ethyl acetate. The organic layer was washed with a saturated sodium bicarbonate aqueous solution and dried over magnesium sulfate, and after concentrated, the residue was purified by flash chromatography on silica gel (n-hexane:ethyl acetate=1:1) and the title compound (6.1 g) was obtained.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07803801B2 |
| Source dataset | uspto-grants-2010_09 |
| ORD ID | ord-c42a456d052b44ef8e071b9acb57adb5 |
| Source note | uspto-grants-2010_09 |