Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
1-Ethyl-3-(3'-dimethylaminopropyl)carbodiimide → 6-Chloro-N-(2-cyclopropylethyl)pyridazine-3-carboxamide
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 1-Ethyl-3-(3'-dimethylaminopropyl)carbodiimide | HCID 15908 | — |
| 반응물 | Diisopropylethylamine | HCID 81531 | — |
| 반응물 | 1-Hydroxybenzotriazole hydrate | HCID 2796029 | — |
| 반응물 | 6-chloropyridazine-3-carboxylic Acid | HCID 6415762 | — |
| 반응물 | Cyclopropaneethanamine | HCID 10240761 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 6-Chloro-N-(2-cyclopropylethyl)pyridazine-3-carboxamide | HCID 65561565 | 55.1% |
반응 단계
To a solution of 6-chloropyridazine-3-carboxylic acid (15.8 mmol) in dichloromethane (95 mL) was added diisopropylethylamine (46.7 mmol), 1-hydroxybenzotriazole monohydrate (23.7 mmol) and 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide (23.7 mmol) under nitrogen atmosphere at ambient temperature. The resulting mixture was stirred for 15 minutes and 2-cyclopropylethylamine (20.2 mmol) was added. After stirring for 36 hours at ambient temperature, the reaction mixture was diluted with dichloromethane (100 mL), then washed with water and dried over anhydrous Na2SO4. The solvent was removed in vacuo. Purification via column chromatography (30% ethyl acetate in hexanes) afforded the title compound (8.70 mmol). Yield 55%.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07951805B2 |
| 출처 데이터셋 | uspto-grants-2011_05 |
| ORD ID | ord-62c5194e7110425d9987a6e1e8cd4d55 |
| 출처 메모 | uspto-grants-2011_05 |