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Hydrochloric Acid → 5-Methylbenzimidazolone
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Water | HCID 962 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | 2-Amino-5-methylbenzoic acid | HCID 76255 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 溶媒 | P,P-Diphenylphosphinic azide | HCID 199401 | — |
| 生成物 | 5-Methylbenzimidazolone | HCID 223134 | — |
反応手順
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.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07772285B2 |
| 出典データセット | uspto-grants-2010_08 |
| ORD ID | ord-fab17d724e3842a1b89b8960d73c792c |
| 出典メモ | uspto-grants-2010_08 |