Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Water → 2,3,4,5-tetrahydro-1H-1-benzazepine-2,5-dione
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | Ethyl 4-(2-aminophenyl)-4-oxobutanoate | HCID 21283602 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 2,3,4,5-tetrahydro-1H-1-benzazepine-2,5-dione | HCID 369398 | 81% |
반응 단계
To a suspension of sodium hydride (10 mg, 0.43 mmol) in dry THF (1 mL) was added 4-(2-amino-phenyl)-4-oxo-butyric acid ethyl ester (80 mg, 0.36 mmol) under Argon at −40° C. The reaction mixture was then allowed to warm up to rt over 3 h, and then added to water (20 mL). The mixture was then extracted with DCM (3×15 mL) and the combined extracts were then dried (sodium sulfate), and evaporated to leave an off-white solid. Recrystallization from EtOAc afforded a white solid (51 mg, 81%), m/z 175 (M).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US06686352B2 |
| 출처 데이터셋 | uspto-grants-2004_02 |
| ORD ID | ord-5ea0ac506de94e1ca90453849bbf16c6 |
| 출처 메모 | uspto-grants-2004_02 |