HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → 1-{3-[2-Chloro-4-(2,4-difluoro-phenylamino)-benzoyl]-4-methyl-phenyl}-1H-[1,2,3]triazole-4-carboxylic acid
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Lithium Hydroxide | HCID 3939 | — |
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | 1-{3-[2-Chloro-4-(2,4-difluoro-phenylamino)-benzoyl]-4-methyl-phenyl}-1H-[1,2,3]triazole-4-carboxylic acid methyl ester | HCID 11540295 | — |
| Catalyst | Hydrochloric Acid | HCID 313 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | 1-{3-[2-Chloro-4-(2,4-difluoro-phenylamino)-benzoyl]-4-methyl-phenyl}-1H-[1,2,3]triazole-4-carboxylic acid | HCID 11525651 | — |
Reaction Steps
A suspension of compound 132 (100 mg, 0.21 mmol) in MeOH (5.0 mL) was added H2O (0.6 mL) and LiOH (25 mg, 1.0 mmol) and the resulting reaction mixture was refluxed for 1 h. EtOAc was added to the reaction and pH adjuste to 1-2 with concentrated HCl (37%, 6 drops). The organic phase was separated and the aqueous layer was extracted with more EtOAc. The organic phases were collected and washed with water, brine, dried (MgSO4), filtered and concentrated in vacuo to give the title compound as white solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08293772B2 |
| Source dataset | uspto-grants-2012_10 |
| ORD ID | ord-76739d4de04f41649d3265a763ce7d95 |
| Source note | uspto-grants-2012_10 |