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HRID 69290作成日:2026年10月25日

Iodine → HCID 57917275、化合物

https://huagongshe.com/reaction/69290

反応式

関与物質

役割名称HCID仕込み量
反応物IodineHCID 807—
反応物Sodium HydroxideHCID 14798—
反応物Phosphinic AcidHCID 4124402—
反応物(Rac)-1-(6-chloro-imidazo[1,2-b]pyridazin-3-yl)-1-(imidazo[1,2-a]pyridin-6-yl)ethanolHCID 87523871—
溶媒Acetic AcidHCID 176—
生成物HCID 57917275HCID 57917275—

反応条件

温度150 °C

反応手順

Iodine (4.8 g, 18.91 mmol) and H3PO2 (5.1 mL of a 50% aqueous solution, 46.8 mmol) were added to a solution of (rac)-1-(6-chloro-imidazo[1,2-b]pyridazin-3-yl)-1-(imidazo[1,2-a]pyridin-6-yl)ethanol (Stage 292.1, 1.85 g, 5.90 mmol) in acetic acid (50 mL). The RM was portion wise in 3 different microwave reactors and was heated at 150° C. for 5 min under microwave irradiations. It was basified with 2.5 N NaOH solution and then it was extracted twice with EtOAc/MeOH (9:1) twice. Combined organic layers was washed with brine and dried over Na2SO4, filtered and concentrated to give the title compound as a brown solid (tR 0.5 min (conditions 2), MH+=298)

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US08822468B2
出典データセットuspto-grants-2014_09
ORD IDord-d015060e79b54a65b317e2272ad33c27
出典メモuspto-grants-2014_09