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Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
HRID 2243767생성일: 2026년 10월 26일

Acetonitrile → 3-[8-(2,6-difluorophenyl)-2-(methylsulfonyl)-7-oxo-5,6,7,8-tetrahydropyrimido[4,5-d]pyrimidin-4-yl]-4-methyl-N-propylbenzamide

https://huagongshe.com/reaction/2243767

반응식

참여 물질

역할이름HCID투입량
반응물AcetonitrileHCID 6342—
반응물3-[8-(2,6-difluorophenyl)-2-(methylthio)-7-oxo-5,6,7,8-tetrahydropyrimido[4,5-d]pyrimidin-4-yl]-4-methyl-N-propylbenzamideHCID 11950263—
반응물Potassium hydroxy sulfiteHCID 23707502—
용매WaterHCID 962—
생성물3-[8-(2,6-difluorophenyl)-2-(methylsulfonyl)-7-oxo-5,6,7,8-tetrahydropyrimido[4,5-d]pyrimidin-4-yl]-4-methyl-N-propylbenzamideHCID 59207990—

반응 단계

To a stirring suspension of Oxone (817.96 g, 1.33 mole, 3 eq) in water (2142 mL, 10 vol) was added 3-[8-(2,6-difluorophenyl)-2-(methylthio)-7-oxo-5,6,7,8-tetrahydropyrimido[4,5-d]pyrimidin-4-yl]-4-methyl-N-propylbenzamide (214.21 g 0.443 mole, 1 eq) suspended in acetonitrile (4284 mL). The resulting mixture was stirred at ambient temperature overnight. The mixture was then filtered and the residue stirred sequentially with 5% sodium metabisulfite (2×3000 mL) and water (1×300 mL). The filtrate from the reaction mixture was then diluted with water (2142 mL, 10 vol). The solid that formed was then collected by filtration. The solid was washed well with water then dried at the pump to yield the title compound. LC-MS m/z 516 (M+H)+, 2.77 min (ret time). It was used without further purification although corresponding sulfoxide was present (about 10%).

출처 및 근거

DOI10.6084/m9.figshare.5104873.v1
특허 번호US07674789B2
출처 데이터셋uspto-grants-2010_03
ORD IDord-76886ac03f234014bb68a8eca88cfe8d
출처 메모uspto-grants-2010_03