Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Methyl iodide | HCID 6328 | — |
| Reactant | Potassium tert-butoxide | HCID 23665647 | — |
| Reactant | HCID 53655223 | HCID 53655223 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 54073603 | HCID 54073603 | 80.3% |
Reaction Steps
First 12.3 g (0.11 mol) of potassium tert.-butanolate and then 15.6 g (0.11 mol) of methyl iodide were added to a solution of 17.6 g (0.1 mol) of 4-methylthioacetoacetic acid ethyl ester in 100 ml of tetrahydrofuran, while cooling. The mixture was subsequently stirred at 60° C. for 12 hours, the solvent was then distilled off in vacuo, 200 ml of methylene chloride were added to the residue and the solution was extracted by shaking twice with 100 ml of water each time. The organic phase was dried over sodium sulphate and evaporated in vacuo. The residue was distilled in vacuo. 14 g (74% of theory) of 2-methyl-4-methylthioacetoacetic acid ethyl ester with a boiling point of 95°-99° C./2 mm Hg were thus obtained. ##STR6##
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US04307107 |
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| Source dataset | uspto-grants-1981_12 |
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| ORD ID | ord-2fa8896017b740c7bba2f770464a2822 |
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| Source note | uspto-grants-1981_12 |
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