HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methyl iodide → 3,6-Dimethylheptane-2,4-dione
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methyl iodide | HCID 6328 | — |
| Reactant | Tetrahydrofuran | HCID 8028 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | 2,4-Heptanedione, 6-methyl- | HCID 76354 | — |
| Solvent | Water | HCID 962 | — |
| Product | 3,6-Dimethylheptane-2,4-dione | HCID 538283 | 94% |
Reaction Steps
To 0.1 mol sodium hydride was added 100 ml anhydrous tetrahydrofuran, then added slowly dropwise 0.1 mol 6-methyl-2,4-heptandione at room temperature. The reaction was stirred for 0.5 hours, then 0.12 mol iodomethane was added dropwise and the reaction was stirred at room temperature for further 10 hours. Upon completing the reaction, 20 ml water was added. The mixture was extracted with ethyl acetate. After removing the solvent, distillation under reduced pressure gave a cut fraction 88-9° C./1 kPa (165-166° C. at atmosphere pressure), and the yield was 94%.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07388061B2 |
| Source dataset | uspto-grants-2008_06 |
| ORD ID | ord-bd5b8d7ad93241e686914bdcd1e363f5 |
| Source note | uspto-grants-2008_06 |