Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Ammonia → 8-Nitro-2,3,4,5-tetrahydro-1H-1-benzazepine
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Ammonia | HCID 222 | — |
| 반응물 | Potassium Nitrate | HCID 24434 | — |
| 반응물 | 2,3,4,5-tetrahydro-1H-1-benzazepine | HCID 576503 | — |
| 용매 | Sulfuric Acid | HCID 1118 | — |
| 생성물 | 8-Nitro-2,3,4,5-tetrahydro-1H-1-benzazepine | HCID 46864071 | 52% |
반응 단계
At −10° C., 2,3,4,5-tetrahydro-1H-benzo[b]azepine (1.9 g, 13 mmol) was added dropwise to a solution of KNO3 (3 g, 30 mmol) in H2SO4 (50 mL). The mixture was stirred for 40 min, poured over crushed ice, basified with aq. ammonia to pH 13, and extracted with EtOAc. The combined organic phases were washed with brine, dried over Na2SO4 and concentrated to give 8-nitro-2,3,4,5-tetrahydro-1H-benzo[b]azepine as a black solid (1.3 g, 51%), which was used without further purification.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08741925B2 |
| 출처 데이터셋 | uspto-grants-2014_06 |
| ORD ID | ord-160f1f7d91a24a0fb92d4a09ca7ffe7e |
| 출처 메모 | uspto-grants-2014_06 |