HuagongsheHuagongshe Chemistry Print Report · For research reference only
Lithium iodide → HCID 15734853, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Lithium iodide | HCID 66321 | — |
| Reactant | HCID 15734813 | HCID 15734813 | — |
| Solvent | Hydrochloric Acid | HCID 313 | — |
| Solvent | 2,6-Lutidine | HCID 7937 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 15734853 | HCID 15734853 | 59.4% |
Reaction Steps
A mixture of ethyl 4-(2-cyanoiminothiazolidin-3-yl)-2,2-dimethyl-2H-1-benzopyran-6-carboxylate (1.15 g) and lithium iodide (3.44 g) in 2,6-lutidine (11.5 ml) was refluxed overnight. The resulting mixture was dissolved in a mixture of ethyl acetate and 10% hydrochloric acid, and the organic layer was separated and washed with brine. The extract was dried over anhydrous magnesium sulfate and concentrated in vacuo. The residue was purified by column chromatography on silica gel (elution with 30:1 to 4:1 chloroform-methanol) followed by recrystallization from ethanol to give 4-(2-cyanoiminothiazolidin-3-yl)-2,2-dimethyl-2H-1-benzopyran-6-carboxylic acid (0.63 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05104890 |
| Source dataset | uspto-grants-1992_04 |
| ORD ID | ord-922fc923eaa7455b8e9bdd34967bc70d |
| Source note | uspto-grants-1992_04 |