HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Carbonate → HCID 15508758, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | Benzoic acid, 4-chloro-3-[(2-chloro-4,4-dimethyl-1,3-dioxopentyl)amino]-, hexadecyl ester | HCID 15476485 | — |
| Reactant | Benzoic acid, 4-hydroxy-3-[(methylsulfonyl)amino]-, methyl ester | HCID 15508757 | — |
| Solvent | Acetone | HCID 180 | — |
| Product | HCID 15508758 | HCID 15508758 | 61% |
Reaction Steps
A suspension of 8.35 g (15 mmol) of 2, 3.68 g (15 mmol) of methyl 4-hydroxy-3-(methanesulfonamido)-benzoate 3 and 6.22 g (45 mmol) of potassium carbonate in 180 mL of acetone was heated at reflux overnight. Thin layer chromatographic analysis indicated reaction was complete. The solvent was removed under vacuum to near dryness, and the residue was treated with a mixture of ethyl acetate and water. The organic liquid phase was washed with dilute hydrochloric acid and then with brine, and then concentrated under vacuum to an oil. The crude product was purified by column chromatography on silica gel using an elution solvent of 30 volume percent ethyl acetate in ligroin. There was thus obtained 7 g (61% yield ) of coupler Y-1.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06162598 |
| Source dataset | uspto-grants-2000_12 |
| ORD ID | ord-e74b7b2eab0349e9bbb774726391f074 |
| Source note | uspto-grants-2000_12 |