HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 18996928, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | p-Toluenesulfonic acid | HCID 6101 | — |
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | HCID 18996925 | HCID 18996925 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | HCID 18996928 | HCID 18996928 | 115.4% |
Reaction Steps
A mixture of t-butyl 2-cyclopropanecarbonyl-3-(2-methylsulphenylpyridin-3-yl)-3-oxopropanoate (9.44 g) and 4-toluenesulphonic acid (0.4 g) in dry toluene was stirred at reflux for 5 hours then allowed to stand at room temperature overnight. The mixture was stirred at reflux for a further 5 hours, cooled to room temperature and taken up into ethyl acetate and water. The phases were separated and the aqueous phase was further extracted with ethyl acetate. The combined organic extracts were dried (anhydrous magnesium sulphate), filtered and evaporated to give 1-cyclopropyl-3-(2-methylsulphenylpyridin-3-yl)propan-1,3-dione (7.64 g) as a brown oil which was used without further purification.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05480857 |
| Source dataset | uspto-grants-1996_01 |
| ORD ID | ord-74671f05ad44411aa328aa3f4bc96e6b |
| Source note | uspto-grants-1996_01 |