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HRID 406200作成日:2026年10月26日

Water → HCID 66665909、化合物

https://huagongshe.com/reaction/406200

反応式

関与物質

役割名称HCID仕込み量
反応物WaterHCID 962—
反応物Potassium PermanganateHCID 516875—
反応物Sodium BisulfiteHCID 23665763—
反応物HCID 66666278HCID 66666278—
触媒Tributylmethylammonium chlorideHCID 91822—
溶媒DichloromethaneHCID 6344—
生成物HCID 66665909HCID 66665909—

反応条件

温度0 °C

反応手順

To a solution of tributylmethylammonium chloride (0.970 g, 4.11 mmol) in DCM (15 ml) at RT under nitrogen was added potassium permanganate (0.650 g, 4.11 mmol) portionwise over 10 minutes. The mixture was cooled to 0° C. and treated dropwise with a solution of tert-butyl 2,3-dip-tolylpyrido[2,3-b]pyrazine-5(6H)-carboxylate (step 2) (1 g, 2.418 mmol) in DCM (10 ml). A solution of sodium bisulfite (1.510 g, 14.51 mmol) in water (12.5 ml) was added keeping the temperature <10° C. The mixture was filtered through Celite® (filter material), washing with DCM. The phases were separated and the organic portion was washed with brine, dried (sodium sulphate), filtered and the solvent was removed in vacuo. The crude product was dissolved in DCM and purified by chromatography on silica eluting with 30-50% EtOAc in iso-hexanes to afford the title compound;

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US08754085B2
出典データセットuspto-grants-2014_06
ORD IDord-5e2b1906b94441489d4cd006247cd8ce
出典メモuspto-grants-2014_06