Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Tin atom | HCID 5352426 | — |
| Reactant | HCID 15457076 | HCID 15457076 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 15457077 | HCID 15457077 | 90% |
Reaction Steps
8.0 g (23 mmol) of 3-(2-chloro-4-hydroxy-5-nitrophenyl)-1-methyl-6-trifluoromethyl-2(1H)-pyridone and 8.2 g (69 mmol) of tin were added to 100 ml of ethanol, and 5 ml of concentrated hydrochloric acid was added thereto under stirring at room temperature, followed by stirring for 1 hour. After completion of the reaction, excess ethanol was distilled off, and the residue was neutralized with a saturated sodium hydrogencarbonate aqueous solution and then extracted with ethyl acetate. The organic layer was washed with water and dried over anhydrous magnesium sulfate. The organic layer was distilled off under reduced pressure to obtain 6.5 g (yield: 90%) of the desired product. 1H-NMR (300 MHz, CDCl3) δ value: 3.74(3H,s), 6.83(1H,d), 7.23(1H,d), 7.30(1H,d), 7.57(1H,d)ppm.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US06265349B1 |
|---|
| Source dataset | uspto-grants-2001_07 |
|---|
| ORD ID | ord-8be61c11e1354dc2a9263d423326f964 |
|---|
| Source note | uspto-grants-2001_07 |
|---|