HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 19777569, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Pinacolone | HCID 6416 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | Dimethyl 4-methoxyisophthalate | HCID 89938 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 19777569 | HCID 19777569 | 66.3% |
Reaction Steps
In a 100 ml three-necked flask equipped with a mechanical stirrer, dropping funnel, reflux condenser, and a nitogen-inlet tube, 1.5 gm (38 mmol) of 60% sodium hydride, 3.6 gm (36 mmol) of pinacolone, 3.0 gm (13.4 mmol) of dimethyl 4-methoxyisophthalate, and 30 ml of anhydrous tetrahydrofuran were mixed with stirring under nitrogen stream and refluxed with heating for 5 hours. After cooling the reaction mixture, 10 ml of 2N aqueous hydrochloric acid was added, and the product was extracted with chloroform. The extract was dried over anhydrous sodium sulfate and the solvent was removed by evaporation. The crude product was recrystallized using hexane to obtain 3.2 gm of the target compound as colorless crystals (yield: 66%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05146002 |
| Source dataset | uspto-grants-1992_09 |
| ORD ID | ord-cb468caedd064eada36d2aabf6216198 |
| Source note | uspto-grants-1992_09 |