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HRID 334437作成日:2026年10月25日

Trifluoroacetic acid → HCID 89465782、化合物

https://huagongshe.com/reaction/334437

反応式

関与物質

役割名称HCID仕込み量
反応物Trifluoroacetic acidHCID 6422—
反応物4-(4-Methylpiperazin-1-yl)benzaldehydeHCID 736533—
反応物Sodium triacetoxyborohydrideHCID 5049666—
反応物HCID 178509236HCID 178509236—
溶媒DichloromethaneHCID 6344—
溶媒TetrahydrofuranHCID 8028—
生成物HCID 89465782HCID 89465782—

反応手順

41.5 μl of trifluoroacetic acid (0.539 mmol) and, in small fractions, 129 mg (0.611 mmol) of sodium triacetoxyborohydride are added to a solution of 100 mg (0.35 mmol) of 5-(3,5-difluorophenylthio)-1H-pyrazolo[3,4-b]pyridin-3-amine and 81 mg (0.395 mmol) of 4-(4-methylpiperazin-1-yl)benzaldehyde in 20 ml of a 1:1 mixture of dichloromethane and tetrahydrofuran. The reaction medium is stirred for 16 hours at room temperature. An additional fraction of 125 μl of trifluoroacetic acid and 388 mg of sodium triacetoxyborohydride are added and the reaction medium is stirred for an additional 24 hours. The solvent is then concentrated and the reaction medium extracted with ethyl acetate and washed using saturated sodium bicarbonate solution. The organic phases are combined, dried on magnesium sulfate and then concentrated to yield a yellow oil. A trituration of this oil in methanol leads to the isolation of 135 mg of a yellow solid.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US08883821B2
出典データセットuspto-grants-2014_11
ORD IDord-989af7569fa646248dd773bdda084e66
出典メモuspto-grants-2014_11