HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 86659403, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | Pyridine, 2,4,6-trichloro- | HCID 27665 | — |
| Reactant | Cyclopropanemethanol | HCID 75644 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 86659403 | HCID 86659403 | 40.3% |
Reaction Steps
109 mg of cyclopropylcarbinol was dissolved in 2 ml of dimethylformamide, and 60 mg of 60% sodium hydride was added thereto under ice water cooling, and the mixture was stirred at room temperature for 20 minutes. To the reaction solution was added 400 mg of 2,4,6-trichloropyridine, and stirred at room temperature for 30 minutes. The reaction solution was added with water and subjected to extraction with ethyl acetate. The organic layer was washed with brine, and then dried over magnesium sulfate. The solvent was distilled off under reduced pressure, and then the obtained residue was purified by silica gel column chromatography to obtain 133 mg of the objective compound as colorless oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08586591B2 |
| Source dataset | uspto-grants-2013_11 |
| ORD ID | ord-af00221d244042c595ffcd44b644ad58 |
| Source note | uspto-grants-2013_11 |