Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Triethylamine → 2-chloro-N-(5-ethyl-1,3,4-oxadiazol-2-yl)-6-(trifluoromethyl)nicotinamide
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | Propylphosphonic anhydride | HCID 111923 | — |
| 반응물 | 5-Ethyl-1,3,4-oxadiazol-2-amine | HCID 343487 | — |
| 반응물 | 2-Chloro-6-(trifluoromethyl)nicotinic acid | HCID 2778210 | — |
| 촉매 | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 2-chloro-N-(5-ethyl-1,3,4-oxadiazol-2-yl)-6-(trifluoromethyl)nicotinamide | HCID 86712495 | — |
반응 단계
200 mg (0.887 mmol) of 2-chloro-6-(trifluoromethyl)nicotinic acid and 100 mg (0.887 mmol) of 5-ethyl-1,3,4-oxadiazol-2-amine are dissolved at RT in 8 ml of CH2Cl2. Then 846 mg (1.33 mmol) of 2,4,6-tripropyl-1,3,5,2,4,6-trioxatriphosphinane 2,4,6-trioxide (50% solution in THF) are added, the mixture is stirred at RT for one hour and then 0.618 ml (4.43 mmol) of triethylamine, 22 mg (0.177 mmol) of 4-dimethylaminopyridine are added. The reaction mixture is stirred at RT for 20 h and then washed twice with 4 ml each time of water, dried over sodium sulfate and concentrated. The residue is purified by column chromatography (prep. HPLC; acetonitrile/water). Yield 80 mg (28%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US09101141B2 |
| 출처 데이터셋 | uspto-grants-2015_08 |
| ORD ID | ord-3314f49db5f94175a762261a6a9c71c7 |
| 출처 메모 | uspto-grants-2015_08 |