HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methyl 4-chloroacetoacetate → HCID 178500938, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methyl 4-chloroacetoacetate | HCID 36240 | — |
| Reactant | Potassium tert-butoxide | HCID 23665647 | — |
| Reactant | HCID 178527894 | HCID 178527894 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 178500938 | HCID 178500938 | 83.5% |
Reaction Steps
Add dropwise potassium tert-butoxide (11.4 g, 101.8 mmol) in 30 ml N,N-dimethylformamide (30 ml) to a solution of [1,2,4]triazole-3-thiol (10.3 gm, 101.8 mmol) in N,N-dimethylformamide (50 ml). Add dropwise methyl 4-chloroacetoacetate (15.3 gm, 101.8 mmol) in N,N-dimethylformamide (15 ml) and stir for 3 hours. Concentrate under reduced pressure, dilute with ethyl acetate (500 ml), filter, and concentrate under reduced pressure. Subject the residue to silica gel chromatography to provide the desired compound (18.3 gm, 83%) as a yellow oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08058425B2 |
| Source dataset | uspto-grants-2011_11 |
| ORD ID | ord-987f6e3f702448f69ef478c522c278cf |
| Source note | uspto-grants-2011_11 |