HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Carbonate → HCID 68816406, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | 1-Iodopropane | HCID 33643 | — |
| Reactant | 1,3-Benzenedicarboxylic acid, 5-hydroxy-, 1,3-dimethyl ester | HCID 83065 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 68816406 | HCID 68816406 | — |
Reaction Steps
Heat commercially available 5-hydroxy-isophthalic acid dimethyl ester (1.0 g, 4.8 mmol), potassium carbonate (5.25 g, 38 mmol) and iodopropane (1.36 g, 8.0 mmol) in DMF (20 mL) at 70° C. for 8 h. Cool to room temperature, partition between ethyl acetate and 10% aqueous potassium carbonate. Wash the ethyl acetate layer with 1 N lithium chloride, saturated aqueous sodium chloride, dry (magnesium sulfate) and concentrate. Dissolve the residue in acetone (10 mL) and add a solution of NaOH (192 mg, 4.80 mmol) in methanol (2 mL). Stir at room temperature 16 h and concentrate. Partition between diethyl ether and 0.1 N citric acid, dry (magnesium sulfate) and concentrate to give the title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07585885B2 |
| Source dataset | uspto-grants-2009_09 |
| ORD ID | ord-dc6438ae10f24edcb974ea95c17370ba |
| Source note | uspto-grants-2009_09 |