HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Lithium hydroxide, monohydrate → 2-(Phenylamino)terephthalic acid
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Lithium hydroxide, monohydrate | HCID 168937 | — |
| Edukt | Dimethyl 2-anilinobenzene-1,4-dicarboxylate | HCID 16748523 | — |
| Lösungsmittel | Methanol | HCID 887 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Lösungsmittel | Tetrahydrofuran | HCID 8028 | — |
| Produkt | 2-(Phenylamino)terephthalic acid | HCID 11448256 | 96% |
Reaktionsschritte
A mixture of compound 1A (4.56 g, 16.0 mmol) and lithium hydroxide monohydrate (2.0 g, 48.0 mmol) in MeOH (32 mL), THF (32 mL) and water (16 mL) was heated to reflux for 0.5 h. HPLC indicated that the reaction was complete. The organic solvents were removed under reduced pressure, and the aqueous residue was diluted with water. The pH was adjusted to 3.0 with 6N aqueous hydrochloric acid. The resulting precipitate was collected by vacuum filtration, rinsed with water and dried under reduced pressure to provide 3.95 g (96%) of 1B as a bright yellow solid. HPLC retention time=2.75 min. (Condition A) and LC/MS M++1=258+.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07312209B2 |
| Quelldatensatz | uspto-grants-2007_12 |
| ORD ID | ord-99b5d171484642b2acb4db020969c60d |
| Quellennotiz | uspto-grants-2007_12 |