HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 70873034, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Diethyl Ether | HCID 3283 | — |
| Reactant | Lithium Chloride | HCID 433294 | — |
| Reactant | HCID 70914950 | HCID 70914950 | — |
| Solvent | Dimethyl Sulfoxide | HCID 679 | — |
| Product | HCID 70873034 | HCID 70873034 | — |
Reaction Steps
3.38 g (10.81 mmol) of dimethyl [2-(4-chlorophenyl)-3-methylbutan-2-yl]malonate, 0.92 g (21.61 mmol) of lithium chloride and 0.2 ml of water in 10 ml of DMSO were heated under reflux for 4 h. After cooling, about 50 ml of diethyl ether were added to the reaction solution, and the phases were separated. The organic phase was washed twice with water, dried over magnesium sulphate and concentrated under reduced pressure. The crude product was purified by chromatography on silica gel (mobile phase cyclohexane/ethyl acetate 10:1). This gave 2.3 g (84% of theory) of the target compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08796335B2 |
| Source dataset | uspto-grants-2014_08 |
| ORD ID | ord-7b8d35e025f743a5aed8be94412ddee0 |
| Source note | uspto-grants-2014_08 |