HuagongsheHuagongshe Chemistry Print Report · For research reference only
Citric Acid → HCID 57901702, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Citric Acid | HCID 311 | — |
| Reactant | Methanol | HCID 887 | — |
| Reactant | Potassium Hydroxide | HCID 14797 | — |
| Reactant | HCID 57476231 | HCID 57476231 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 57901702 | HCID 57901702 | 99.5% |
Reaction Steps
To a mixed solution of ethyl 5-methyl-7-[(2-thienylsulfonyl)amino]-1H-indole-2-carboxylate (0.80 g) in tetrahydrofuran (15 mL)-methanol (15 mL) was added aqueous solution (5 mL) of 85% potassium hydroxide (0.65 g), and the mixture was stirred at room temperature for 15 hr. Aqueous citric acid solution was added to the reaction mixture, and the mixture was extracted with ethyl acetate, washed with saturated brine, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The obtained crystals were washed with ethyl acetate-hexane to give the title compound (735 mg, yield 99%) as pale-yellow crystals. melting point>280° C. (decomposition).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08957070B2 |
| Source dataset | uspto-grants-2015_02 |
| ORD ID | ord-1c980f094e914f14b25311efa7db8b08 |
| Source note | uspto-grants-2015_02 |