HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 58288282, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Diethyl Ether | HCID 3283 | — |
| Reactant | Lithium Chloride | HCID 433294 | — |
| Reactant | HCID 58288432 | HCID 58288432 | — |
| Solvent | Dimethyl Sulfoxide | HCID 679 | — |
| Product | HCID 58288282 | HCID 58288282 | — |
Reaction Steps
A solution of 796 mg (2.55 mmol) of diethyl [2-(4-chlorophenyl)propan-2-yl]malonate, 216 mg (5.10 mmol) of lithium chloride and 46 μl (2.55 mmol) of water in 5 ml of DMSO was heated to reflux and stirred at this temperature for 4 h. After cooling to room temperature, 20 ml of diethyl ether and 20 ml of water were added to the reaction mixture. After separation of the phases, the organic phase was washed three more times with water, and the organic phase was dried over magnesium sulphate and then concentrated to dryness. The crude product was purified by preparative HPLC (mobile phase methanol/water 70:30). This gave 276 mg of the title compound (45% of theory).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09018414B2 |
| Source dataset | uspto-grants-2015_04 |
| ORD ID | ord-7c0882a1fdd44c1e96594d40bae7f3a9 |
| Source note | uspto-grants-2015_04 |