돌아가기
Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
HRID 49669생성일: 2026년 10월 26일

Triethylamine → HCID 178428868, 화합물

https://huagongshe.com/reaction/49669

반응식

참여 물질

역할이름HCID투입량
반응물TriethylamineHCID 8471—
반응물Potassium CarbonateHCID 11430—
반응물3-(3-Bromo-2-methyl-6-(methylsulfonyl)phenyl)-4,5-dihydroisoxazoleHCID 10947075—
반응물HCID 178481816HCID 178481816—
촉매HCID 178418476HCID 178418476—
용매1,4-DioxaneHCID 31275—
생성물HCID 178428868HCID 17842886811.1%

반응 조건

온도130 °C

반응 단계

2.2 l of 1,4-dioxane, 100 g (0.315 mol) of 3-(3-bromo-2-methyl-6-methylsulfonylphenyl)-4,5-dihydroisoxazole, 30.82 g (0.315 mol) of 1-methyl-5-hydroxypyrazole, 87 g (0.63 mol) of potassium carbonate, 63.5 g (0.63 mol) of triethylamine and 11.2 g (0.016 mol) of bis(triphenylphosphine)-palladium dichloride were added to a 3.5 l autoclave. The autoclave was then flushed twice with nitrogen, a carbon monoxide pressure of 10 kg/cm2 was applied and the mixture was heated with stirring to 130° C. The carbon monoxide pressure was increased to 20 kg/cm2 and the mixture was stirred at 130° C. for 24 h. The mixture was then concentrated under reduced pressure and the residue was taken up in water. The aqueous phase of pH 11 was extracted with dichloromethane. The organic phase is discarded. The aqueous phase is adjusted to pH 4 using 18% strength hydrochloric acid. The precipitate was filtered off, washed three times with water and dried at 40° C. under reduced pressure. This gives 85 g of product. The filtrate is extracted with dichloromethane. The organic phase is dried with sodium sulfate, and the solvent is then removed under reduced pressure, giving a further 12.7 g of product.

출처 및 근거

DOI10.6084/m9.figshare.5104873.v1
특허 번호US06706886B2
출처 데이터셋uspto-grants-2004_03
ORD IDord-b10cfe3058f944dc843a68922384baae
출처 메모uspto-grants-2004_03