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HRID 45862作成日:2026年10月23日

Gamma-Butyrolactone → HCID 178520695、化合物

https://huagongshe.com/ja/reaction/45862

反応式

関与物質

役割名称HCID仕込み量
反応物Gamma-ButyrolactoneHCID 7302—
反応物Sodium hexamethyidisilazaneHCID 45051731—
反応物HCID 178507322HCID 178507322—
溶媒TetrahydrofuranHCID 8028—
生成物HCID 178520695HCID 17852069559%

反応条件

温度0 °C

反応手順

30 mg (0.068 mmol) of 1-{3-[4-(2-aminopyridin-4-yl)-1H-pyrazol-3-yl]phenyl}-3-[4-(trifluoromethyl)phenyl]urea were dissolved in 2 ml of dry tetrahydrofuran and 15 μl (0.34 mmol) of γ-butyrolactone were added. The reaction mixture was cooled to 0° C. and a solution of 680 μl (0.68 mmol) of hexamethyldisilazane sodium salt 1M in THF in 2 ml of the same solvent were added dropwise. The mixture was maintained at 0° C. for 6 hours and at room temperature overnight, then partitioned between dichloromethane and water. The organic phase was dried over sodium sulphate and evaporated. The crude was finally purified by preparative HPLC in reverse phase conditions (basic eluant), giving 20 mg (59%) of the title compound.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US08541575B2
出典データセットuspto-grants-2013_09
ORD IDord-3cff4afe910941b08835c59a82d566ad
出典メモuspto-grants-2013_09