HuagongsheHuagongshe Chemistry Print Report · For research reference only
4-Hydroxybenzaldehyde → HCID 58284274, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 4-Hydroxybenzaldehyde | HCID 126 | — |
| Reactant | Sodium Carbonate | HCID 10340 | — |
| Reactant | 1-Chloro-2-methylpropan-2-ol | HCID 68409 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 58284274 | HCID 58284274 | — |
Reaction Steps
5.00 g (40.94 mmol) of 4-hydroxybenzaldehyde, 4.44 g (40.94 mmol) of 1-chloro-2-methyl-2-propanol and 6.08 g (57.32 mmol) of sodium carbonate are initially charged in 50 ml of dry DMF and stirred under reflux for 24 h. After cooling to RT, 20 ml of ethyl acetate and 20 ml of sat. aqueous sodium bicarbonate solution are added. The phases are separated, and the organic phase is dried over magnesium sulfate. After removal of the solvent, the residue is purified by column chromatography on silica gel 60 (mobile phase gradient: cyclohexane/ethyl acetate 5:1→1:1). This gives a reddish solid which is used without further purification for the subsequent step.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09095582B2 |
| Source dataset | uspto-grants-2015_08 |
| ORD ID | ord-5b55655856154b78a9f3cbfd51962cfd |
| Source note | uspto-grants-2015_08 |