참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | Pyridine | HCID 1049 | — |
| 반응물 | 4-Chloroaniline | HCID 7812 | — |
| 반응물 | 5-Bromo-pyridine-2-carbonyl chloride | HCID 19090771 | — |
| 촉매 | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Acetonitrile | HCID 6342 | — |
| 생성물 | 5-Bromo-pyridine-2-carboxylic acid (4-chloro-phenyl)-amide | HCID 59593371 | — |
반응 단계
To 5-Bromo-pyridine-2-carbonyl chloride (69, 0.76 g, 3.4 mmol) in acetonitrile (29.0 mL) were added p-chloroaniline (53, 0.702 g, 5.50 mmol), 4-dimethylamino-pyridine (0.12 g, 0.96 mmol) and pyridine (2.9 mL, 0.036 mol). The reaction was stirred at 68° C. overnight, then poured into water, acidified with 1N HCl to pH around 1 and extracted with ethyl acetate. The organic layer was dried over anhydrous sodium sulfate and filtered. The filtrate was concentrated and purified by silica gel column chromatography eluting with dichloromethane to give a white solid (70, 0.75 g, 70.0%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US08722702B2 |
|---|
| 출처 데이터셋 | uspto-grants-2014_05 |
|---|
| ORD ID | ord-8d55364b25e644b4a76c53b27d8e02a8 |
|---|
| 출처 메모 | uspto-grants-2014_05 |
|---|