HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → 4-(4-Chlorophenyl)-2-methoxybenzoic acid
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Lithium Hydroxide | HCID 3939 | — |
| Reactant | 4'-Chloro-3-methoxy-biphenyl-4-carboxylic acid methyl ester | HCID 59513082 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | 4-(4-Chlorophenyl)-2-methoxybenzoic acid | HCID 24891199 | 91% |
Reaction Steps
To a solution of 4′-chloro-3-methoxy-biphenyl-4-carboxylic acid methyl ester, 8, (0.615 g, 2.22 mmol) in THF (20 mL) and H2O (5 mL) at room temperature is added LiOH (0.932 g, 22.2 mmol). The resulting suspension is heated to reflux for 2 hours. The reaction is cooled and concentrated under reduced pressure. The crude product is acidified using conc. HCl and the resulting solid is collected by filtration washed with H2O and dried to afford 0.532 g (91%) of the desired product as a grey solid. 1H NMR (400 MHz, CDCl3) δ ppm 10.69 (1H, br s), 8.26 (1H, d, J=8.1 Hz), 7.53-7.58 (2H, m), 7.44-7.50 (2H, m), 7.33 (1H, dd, J=8.1, 1.6 Hz), 7.20 (1H, d, J=1.3 Hz), 4.17 (3H, s). HPLC-MS: m/z 263 [M+H]+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08598210B2 |
| Source dataset | uspto-grants-2013_12 |
| ORD ID | ord-bdf4b751d85446bc86080f4c617e8f8b |
| Source note | uspto-grants-2013_12 |