참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Sodium Iodide | HCID 5238 | — |
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | 6-Chloropyridazin-3-ol | HCID 252828 | — |
| 반응물 | N,N-Dimethylaminoethyl chloride hydrochloride | HCID 11636816 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | 6-Chloro-2-(2-(dimethylamino)ethyl)pyridazin-3(2H)-one | HCID 69306583 | 22.5% |
반응 단계
To a solution of 6-chloro-2H-pyridazin-3-one (500 mg, 3.83 mmol) in 5 mL dimethylformamide was added 2-dimethylaminoethyl chloride hydrochloride (828 mg, 5.75 mmol), potassium carbonate (1.59 g, 11.5 mmol) and sodium iodide (632 mg, 4.21 mmol). The mixture was stirred over night at 65° C. Solvent was evaporated. The crude product was dissolved in water and purified by preparative HPLC using a gradient of acetonitrile/5% acetonitrile—water phase containing 0.1 M ammonium acetate, to give 174 mg of 6-chloro-2-(2-dimethylamino-ethyl)-2H-pyridazin-3-one as light brown crystals after freeze drying (22% yield).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US07419979B2 |
|---|
| 출처 데이터셋 | uspto-grants-2008_09 |
|---|
| ORD ID | ord-f9aa938a188a4e96a702ce5c78b1c47e |
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| 출처 메모 | uspto-grants-2008_09 |
|---|
