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HRID 577615作成日:2026年10月25日

Sodium Hydroxide → 6-Iodobenzo[d][1,3]dioxol-5-amine

https://huagongshe.com/reaction/577615

反応式

関与物質

役割名称HCID仕込み量
反応物Sodium HydroxideHCID 14798—
反応物N-(6-Iodo-2H-1,3-benzodioxol-5-yl)acetamideHCID 53488067—
溶媒EthanolHCID 702—
溶媒WaterHCID 962—
生成物6-Iodobenzo[d][1,3]dioxol-5-amineHCID 5348806898.5%

反応手順

A solution of N-(6-iodobenzo[d][1,3]dioxol-5-yl)acetamide (200 mg, 0.656 mmol) and NaOH (1.31 g, 32.8 mmol) in ethanol (26 mL) and water (6 mL) was heated to reflux with stirring for 4 h. The mixture was cooled and the solvent was removed under vacuum. The residue was partitioned between methylene chloride (100 mL) and water (100 mL). The organic layer was washed with water (2×100 mL), dried (MgSO4) and evaporated under vacuum to give 6-iodobenzo[d][1,3]dioxol-5-amine (170 mg, 98%) as orange solid. LCMS: 264 [M+1]+; 1H NMR (DMSO-d6) δ 4.88 (s, 2H), 5.87 (s, 2H), 6.47 (s, 1H), 7.07 (s, 1H).

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US09040556B2
出典データセットuspto-grants-2015_05
ORD IDord-6737bf79289e43c6b64daca6dbf42d36
出典メモuspto-grants-2015_05