HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Hydrochloric Acid → 5-Methylbenzimidazolone
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Hydrochloric Acid | HCID 313 | — |
| Edukt | Water | HCID 962 | — |
| Edukt | Triethylamine | HCID 8471 | — |
| Edukt | Ethyl Acetate | HCID 8857 | — |
| Edukt | 2-Amino-5-methylbenzoic acid | HCID 76255 | — |
| Lösungsmittel | 1,4-Dioxane | HCID 31275 | — |
| Lösungsmittel | P,P-Diphenylphosphinic azide | HCID 199401 | — |
| Produkt | 5-Methylbenzimidazolone | HCID 223134 | — |
Reaktionsschritte
4.00 g of 2-amino-5-methylbenzoic acid was dissolved in 40 mL of 1,4-dioxane, to which 5.5 mL of triethylamine and 6.8 mL of diphenylphosphoryl azide were successively added, and this mixture was stirred for 1.5 hours while heating it under reflux. The reaction mixture, to which a mixture of ethyl acetate and water was added, was adjusted to pH 7 with 1M hydrochloric acid, and the organic phase was separated therefrom. After the resultant organic phase was washed with water and a saturated sodium chloride solution successively, the washed phase was dried over anhydrous sodium sulfate, and the solvent was distilled out under reduced pressure to yield 2.96 g of 5-methyl-1,3-dihydro-2H-benzimidazol-2-one as light yellow solid.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07772285B2 |
| Quelldatensatz | uspto-grants-2010_08 |
| ORD ID | ord-fab17d724e3842a1b89b8960d73c792c |
| Quellennotiz | uspto-grants-2010_08 |