HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 70128654, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Chloromethyl Methyl Ether | HCID 7864 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | HCID 70128516 | HCID 70128516 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 70128654 | HCID 70128654 | 86.5% |
Reaction Steps
992 mg of 1-benzyl 3-tert-butyl 2-ethyl 1-oxo-1,2,3-propanetricarboxylate in 10 ml of dimethylformamide was stirred together with 131 mg of 60% oily sodium hydride at room temperature for 1 hour. After addition of 273 mg of chloromethyl methyl ether, the reaction solution was stirred for another 45 minutes, then poured into water and extracted with ethyl ether. The organic layer was dried over anhydrous magnesium sulfate. The desiccant was filtered off, and the solvent was distilled off under reduced pressure. The residue was purified by silica gel column chromatography [hexane/ethyl acetate=5/1] to give 962 mg of the title compound as a colorless oily substance.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06048894 |
| Source dataset | uspto-grants-2000_04 |
| ORD ID | ord-a644a88ec2a34367ae92256443a10656 |
| Source note | uspto-grants-2000_04 |