Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | Potassium bisulfate | HCID 516920 | — |
| Reactant | Aluminium lithium hydride | HCID 21226445 | — |
| Reactant | HCID 67081820 | HCID 67081820 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 67081917 | HCID 67081917 | 136.9% |
Reaction Steps
10 ml of lithium aluminium hydride (1 M in tetrahydrofuran) are introduced into a three-necked flask under argon. After having cooled the solution to 0° C., 1.0 g (3.2 mmol) of diethyl 2,2′-[(5-methoxy-1,3-phenylene)bis(oxy)]diacetate in solution in 6 ml of tetrahydrofuran is added. The formation of a white precipitate is observed. After stirring for one hour at ambient temperature, ethyl acetate is slowly added at 0° C. The mixture is poured into a saturated aqueous solution of potassium hydrogen sulphate and the mixture is extracted with ethyl acetate. The organic phase is washed with a saturated solution of sodium chloride and dried over sodium sulphate, then concentrated to dryness. 1.0 g (78%) of a white powder is obtained.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US09120819B2 |
|---|
| Source dataset | uspto-grants-2015_09 |
|---|
| ORD ID | ord-afd6c3c6703444c18ed2f937dc693a5d |
|---|
| Source note | uspto-grants-2015_09 |
|---|