Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Citric Acid → 3-cyclopropyl-2-{[2-methyl-6-(1H-1,2,4-triazol-1-yl)-pyridin-3-yl]carbonyl}-3-oxopropanenitrile
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Citric Acid | HCID 311 | — |
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | 3-Cyclopropyl-3-oxopropanenitrile | HCID 9812763 | — |
| 반응물 | 2-methyl-6-(1H-1,2,4-triazol-1-yl)nicotinic acid chloride | HCID 58453090 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 3-cyclopropyl-2-{[2-methyl-6-(1H-1,2,4-triazol-1-yl)-pyridin-3-yl]carbonyl}-3-oxopropanenitrile | HCID 58453106 | 64% |
반응 단계
A THF (2 ml) suspension of sodium hydride (0.06 g, 60% oil suspension, 18.78 mmol) was cooled in an ice bath, and a THF (2 ml) solution of 3-cyclopropyl-3-oxopropanenitrile was dripped thereto. To the obtained reaction solution, a THF (3 ml) solution of 2-methyl-6-(1H-1,2,4-triazol-1-yl)nicotinic acid chloride (0.16 g, 0.73 mmol) was dripped. The resultant was stirred at room temperature for 3 hours. The obtained reaction solution was made acidic with a citric acid aqueous solution, and the product was extracted with ethyl acetate. The obtained organic layer was washed with water, dried with magnesium sulfate and concentrated to obtain the desired product (0.14 g, yield 64%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08927458B2 |
| 출처 데이터셋 | uspto-grants-2015_01 |
| ORD ID | ord-c120433afb5e4c8eaa5b4d6d03b5e644 |
| 출처 메모 | uspto-grants-2015_01 |