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HRID 25459생성일: 2026년 10월 24일

Monoperoxyphthalic Acid Magnesium Salt → 4-Fluoro-1-methylsulfinyl-2-nitrobenzene

https://huagongshe.com/ko/reaction/25459

반응식

참여 물질

역할이름HCID투입량
반응물Monoperoxyphthalic Acid Magnesium SaltHCID 10130449—
반응물4-Fluoro-1-(methylsulfanyl)-2-nitrobenzeneHCID 12700911—
용매MethanolHCID 887—
용매DichloromethaneHCID 6344—
생성물4-Fluoro-1-methylsulfinyl-2-nitrobenzeneHCID 2256734663%

반응 조건

온도20 °C

반응 단계

4-Fluoro-1-methylsulfinyl-2-nitrobenzene can be obtained in the following way: 4.7 g of magnesium monoperoxyphthalate are added portionwise to a solution, under argon, of 1.9 g of 4-fluoro-1-methylsulfanyl-2-nitrobenzene in 6 ml of methanol and 30 ml of dichloromethane. The reaction mixture is then stirred at a temperature in the region of 20° C. for 3 hours, and is then filtered through sintered glass and the solid is washed with dichloromethane. The filtrate is washed with an aqueous sodium hydrogencarbonate solution then with water, dried over magnesium sulfate, treated with 3S black, filtered and then concentrated to dryness under reduced pressure (2 kPa) at a temperature in the region of 40° C. The residue thus obtained is purified by chromatography on a column of 125 g of silice (particle size 40-63 μm), eluting with pure dichloromethane. The fractions containing the expected product are pooled and concentrated to dryness under reduced pressure (2 kPa) at a temperature in the region of 40° C. 1.3 g of 4-fluoro-1-methylsulfinyl-2-nitrobenzene are thus obtained in the form of a yellow foam (Rf=0.23, silica gel thin layer chromatography, eluent: dichloromethane/ethyl acetate 90/10)).

출처 및 근거

DOI10.6084/m9.figshare.5104873.v1
특허 번호US06858638B2
출처 데이터셋uspto-grants-2005_02
ORD IDord-d3701a554f694506a5dba40497c51f19
출처 메모uspto-grants-2005_02