HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Chloride → HCID 56617608, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Chloride | HCID 5234 | — |
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | tert-Butyl 4-chloro-3-oxobutyrate | HCID 2724514 | — |
| Reactant | Potassium ethanethioate | HCID 23670855 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 56617608 | HCID 56617608 | 83% |
Reaction Steps
2.40 g (21.0 mmol) of dry potassium thioacetate were added to a solution, which had been cooled to 0° C., of 3.85 g (20.0 mmol) of tert.-butyl 4-chloroacetoacetate in 40 ml of anhydrous acetonitrile, and the mixture was stirred at this temperature for 30 min. It was then poured into a mixture of NaCl solution and ethyl acetate, the organic phase was separated off, extraction with 2×30 ml of ethyl acetate was carried out, and the extract was washed with water and dried over MgSO4. After evaporation of the solvent in vacuo and chromatography of the residue on 60 g of silica gel (toluene:ethyl acetate 95:5), 3.87 g (83%) of the title compound were obtained as a colorless oil, Rf: 0.24 (toluene:ethyl acetate 95:5).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04841042 |
| Source dataset | uspto-grants-1989_06 |
| ORD ID | ord-8063340909ba4a3fa35af49d5670c993 |
| Source note | uspto-grants-1989_06 |