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Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
HRID 1877507생성일: 2026년 10월 25일

Water → 2-Cyano-5-fluoro-3-(1,2,2,6,6-pentamethylpiperidin-4-yl)aminopyridine

https://huagongshe.com/reaction/1877507

반응식

참여 물질

역할이름HCID투입량
반응물WaterHCID 962—
반응물Ethyl AcetateHCID 8857—
반응물4-Amino-1,2,2,6,6-pentamethylpiperidineHCID 693792—
반응물2-Cyano-3,5-difluoropyridineHCID 2783253—
촉매Potassium CarbonateHCID 11430—
용매Dimethyl SulfoxideHCID 679—
생성물2-Cyano-5-fluoro-3-(1,2,2,6,6-pentamethylpiperidin-4-yl)aminopyridineHCID 5833835320.5%

반응 조건

온도115 °C

반응 단계

682 mg of 2-cyano-3,5-difluoropyridine, 995 mg of 4-amino-1,2,2,6,6-pentamethylpiperidine and 1.346 mg of potassium carbonate in 10 ml of dimethyl sulphoxide are introduced into a 20 ml microwave tube reactor. The mixture is then heated in the microwave for 1 hour at 115° C. The reaction medium is run into 100 ml of water and 100 ml of ethyl acetate. The aqueous phase is re-extracted twice with 50 ml of ethyl acetate. The combined organic phases are washed with water and then with a saturated aqueous solution of sodium chloride, dried over sodium sulphate and concentrated under reduced pressure. After purification by flash chromatography on 70 g of silica gel, elution being carried out with a mixture of dichloromethane, methanol and 4N aqueous ammonia (99/1/0.8 by volume), and the first eluted product being recovered, 290 mg of 2-cyano-5-fluoro-3-(1,2,2,6,6-pentamethylpiperidin-4-yl)aminopyridine are thus obtained in the form of an ecru powder, the characteristics of which are the following:

출처 및 근거

DOI10.6084/m9.figshare.5104873.v1
특허 번호US08309721B2
출처 데이터셋uspto-grants-2012_11
ORD IDord-ebbd255367b446169d7e52e2837024fa
출처 메모uspto-grants-2012_11