Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | Ethyl 4-cyanobenzoate | HCID 81589 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | 4-Cyanobenzoic acid | HCID 12087 | 80.2% |
Reaction Steps
A mixture containing ethyl p-cyanobenzoate (87.5 g, 0.5 mol), water (320.8 g), and methanol (320.8 g) was placed in a 1 l-flask. The mixture was heated to 80° C. with stirring by use of a mechanical stirrer. A 20% aqueous solution of sodium hydroxide was added to the mixture so as to adjust the pH of the mixture at 8.0-8.3. Twenty-four hours after the reaction started, liquid chromatographic analysis revealed that the reaction mixture contained 58.9 g of p-cyanobenzoic acid (yield 80.2%). The reaction mixture was cooled to 30° C., and hydrochloric acid was added thereto to lower the pH to 3.1. The mixture was heated again to 82° C. to dissolve. The resultant mixture was cooled for crystallization, to thereby obtain 57.7 g of p-cyanobenzoic acid crystal (purity 96.8%, yield 76%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US06433211B1 |
|---|
| Source dataset | uspto-grants-2002_08 |
|---|
| ORD ID | ord-d9c442f99d8d45b9a471fac9d07f1a91 |
|---|
| Source note | uspto-grants-2002_08 |
|---|