Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Acetic Acid → Methyl 2-((tert-butoxycarbonyl(methyl)amino)methyl)-1H-benzo[d]imidazole-4-carboxylate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Acetic Acid | HCID 176 | — |
| 반응물 | Methyl 2-amino-3-(2-(tert-butoxycarbonyl(methyl)amino)acetamido)benzoate | HCID 58101623 | — |
| 용매 | O-Xylene | HCID 7237 | — |
| 생성물 | Methyl 2-((tert-butoxycarbonyl(methyl)amino)methyl)-1H-benzo[d]imidazole-4-carboxylate | HCID 58101688 | 90% |
반응 단계
Acetic acid (45 ml) was added to a solution of methyl 2-amino-3-(2-(tert-butoxycarbonyl(methyl)amino)acetamido)benzoate (19.28 mmol, 1.0 eq.) in xylene (130 ml) and the reaction mixture was heated under reflux for 1 h. When the reaction was complete (checking by TLC), the solvent was evaporated to dryness, the residue was dissolved in ethyl acetate and the solution was washed with water and NaCl solution. The organic phase was concentrated to dryness in vacuo in order to obtain the desired product, which was employed in the next stage without further purification. Yield: 90%
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08232288B2 |
| 출처 데이터셋 | uspto-grants-2012_07 |
| ORD ID | ord-05311a0fb45a47a68c0875d33fe5e759 |
| 출처 메모 | uspto-grants-2012_07 |