참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Sulfuric Acid | HCID 1118 | — |
| 반응물 | 4-Bromophenylhydrazine hydrochloride | HCID 12157 | — |
| 반응물 | 2,3,4,5-tetrahydro-1H-1-benzazepine-2,5-dione | HCID 369398 | — |
| 반응물 | Sodium Acetate | HCID 517045 | — |
| 용매 | Acetic Acid | HCID 176 | — |
| 생성물 | Kenpaullone | HCID 3820 | 86.3% |
반응 단계
To a suspension of 1H-[1]benzazepin-2,5(3H, 4H)-dione (0.247 g, 1.3 mmol) in acetic acid (5 ml) was added 4-bromophenylhydrazine hydrochloride (0.532 g, 2.3 mmol) and sodium acetate (0.195 g, 2.3 mmol) and stirred under argon. The mixture was heated at 70° C. for 3 hours, then cooled and concentrated sulfuric acid (0.5 ml) added, before heating at 70° C. for a further 3 hours. The slurry was poured into 10% sodium acetate aqueous solution (20 ml) and the precipitate filtered to give the title compound as a cream solid (0.367 g, yield 79.6%), mp>300° C.; 1H-NMR (DMSO-d6, 300 MHz): δ (ppm)=11.82 (s; 1 H), 10.1 (s; 1H), 7.89 (d; 1H), 7.74 (dd; 1H), 7.41-7.36 (m; 2H), 7.30-7.21 (m; 3H), 3.51 (s; 2H).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US07767664B2 |
|---|
| 출처 데이터셋 | uspto-grants-2010_08 |
|---|
| ORD ID | ord-8eeb5fd0bebb403193bc6b4eb854ffd4 |
|---|
| 출처 메모 | uspto-grants-2010_08 |
|---|
