HuagongsheHuagongshe Chemistry Print Report · For research reference only
Citric Acid → HCID 57901861, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Citric Acid | HCID 311 | — |
| Reactant | Methanol | HCID 887 | — |
| Reactant | Potassium Hydroxide | HCID 14797 | — |
| Reactant | HCID 57901632 | HCID 57901632 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 57901861 | HCID 57901861 | 93% |
Reaction Steps
To a mixed solution of ethyl 4-(propylsulfonyl)-7-[(2-thienylsulfonyl)amino]-1H-indole-2-carboxylate (0.56 g) in tetrahydrofuran (15 mL)-methanol (15 mL) was added aqueous solution (5 mL) of 85% potassium hydroxide (0.35 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 oil was crystallized from ethyl acetate-hexane to give the title compound (486 mg, yield 93%) as pale-yellow prism crystals. melting point 247-248° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08957070B2 |
| Source dataset | uspto-grants-2015_02 |
| ORD ID | ord-9b61f12707cd400bb1de7502a70a95c5 |
| Source note | uspto-grants-2015_02 |