Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Nitromethane → 1H-benzimidazol-1-ol 3-oxide
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Nitromethane | HCID 6375 | — |
| 반응물 | 4,6-Dimethylpyrimidine | HCID 15257 | — |
| 반응물 | Benzofuroxan | HCID 68075 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 1H-benzimidazol-1-ol 3-oxide | HCID 12349347 | — |
반응 단계
To a mixture containing nitromethane (7.4 g., 0.12 moles), benzofuroxan 13.6 g., 0.10 moles) and tetrahydrofuran (50 ml.) is slowly added dimethylpyrimidine (11.3 g.) dropwise. The heat of reaction causes the reaction temperature to rise sharply; therefore, an ice-bath is used to maintain a steady rate of reflux. Upon completion of addition, the resulting mixture is allowed to cool to room temperature whereupon the solid product which precipitates is filtered, washed with water, dried and recrystallized from a MeOH/NaOCH3 mixture which is subsequently acidified. The crystalline product has an M.P. 213° C. dec.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US04866175 |
| 출처 데이터셋 | uspto-grants-1989_09 |
| ORD ID | ord-7e53e56e1e234f45b968485bf6b00ec8 |
| 출처 메모 | uspto-grants-1989_09 |