Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Hydrochloric Acid → 5-Methylbenzimidazolone
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | Water | HCID 962 | — |
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | Ethyl Acetate | HCID 8857 | — |
| 반응물 | 2-Amino-5-methylbenzoic acid | HCID 76255 | — |
| 용매 | 1,4-Dioxane | HCID 31275 | — |
| 용매 | P,P-Diphenylphosphinic azide | HCID 199401 | — |
| 생성물 | 5-Methylbenzimidazolone | HCID 223134 | — |
반응 단계
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.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07772285B2 |
| 출처 데이터셋 | uspto-grants-2010_08 |
| ORD ID | ord-fab17d724e3842a1b89b8960d73c792c |
| 출처 메모 | uspto-grants-2010_08 |