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Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
HRID 990237생성일: 2026년 10월 26일

(-)-2-Butanol → 3-Ethyl-5-[5-(4-ethylpiperazin-1-ylsulphonyl)-2-(1(r)-methyl-n-propoxy)pyridin-3-yl]-2-methyl-2,6-dihydro-7h-pyrazolo[4,3-d]pyrimidin-7-one

https://huagongshe.com/reaction/990237

반응식

참여 물질

역할이름HCID투입량
반응물(-)-2-ButanolHCID 84682—
반응물Potassium bis(trimethylsilyl)amideHCID 3251421—
반응물5-[2-Ethoxy-5-(4-ethylpiperazin-1-ylsulphonyl)pyridin-3-yl]-3-ethyl-2-methyl-2,6-dihydro-7h-pyrazolo[4,3-d]pyrimidin-7-oneHCID 135816367—
생성물3-Ethyl-5-[5-(4-ethylpiperazin-1-ylsulphonyl)-2-(1(r)-methyl-n-propoxy)pyridin-3-yl]-2-methyl-2,6-dihydro-7h-pyrazolo[4,3-d]pyrimidin-7-oneHCID 13603645917%

반응 조건

온도110 °C

반응 단계

The title compound of Example 78 (400 mg, 0.84 mmol) was added to a mixture of potassium bis(trimethylsilyl)amide (840 mg, 4.2 mmol) in (R)-2-butanol (4 ml) and the mixture stirred at 110° C. for 18 hours. The cooled mixture was concentrated under reduced pressure and the residue suspended in water (10 ml) and neutralised using 2N hydrochloric acid. This aqueous suspension was extracted with ethyl acetate (3×30 ml), the combined organic extracts washed with sodium hydroxide solution (20 ml), brine (2×30 ml), dried (Na2SO4) and evaporated under reduced pressure. The crude product was purified by column chromatography on silica gel, using an elution gradient of dichloromethane:methanol (100:0 to 97.5:2.5) and the product suspended in ether and evaporated under reduced pressure. This solid was recrystallised from hexane/ethyl acetate to afford the title compound (72 mg, 17%) as a white solid.

출처 및 근거

DOI10.6084/m9.figshare.5104873.v1
특허 번호US06458951B2
출처 데이터셋uspto-grants-2002_10
ORD IDord-984400835fd7410f8231b6c1d08260c0
출처 메모uspto-grants-2002_10