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HRID 1089545作成日:2026年10月27日

Potassium Carbonate → 4-[(4-Methylphenyl)sulfonyl]-9-nitro-3,4,5,6-tetrahydro-2H-1,7,4-benzodioxazonine

https://huagongshe.com/reaction/1089545

反応式

関与物質

役割名称HCID仕込み量
反応物Potassium CarbonateHCID 11430—
反応物N,N-bis(2-(p-toluenesulfonyloxy)ethyl)-p-toluenesulfonamideHCID 267409—
反応物4-NitrocatecholHCID 3505109—
溶媒DimethylformamideHCID 6228—
生成物4-[(4-Methylphenyl)sulfonyl]-9-nitro-3,4,5,6-tetrahydro-2H-1,7,4-benzodioxazonineHCID 14856355—

反応手順

To dimethylformamide (200 mL) add 4-nitrocatechol (13.8 g, 89 mmol), 4-methyl-N,N-bis[2-[[(4-methylphenyl)sulfonyl]oxy]ethyl]benzenesulfonamide (50.7 g, 89.4 mmol), and K2CO3 (27 g, 0.19 mol). Stir and heat the reaction at 110° C. Monitor the progress of the reaction by thin-layer chromatography. Upon completion remove the heat and add water (1.3 L) and methanol (300 mL). Collect the precipitate on paper by suction filtration. Wash the solid with water (2 L). Chromatograph the material on silica (300 g) with CH2Cl2 to obtain the title compound.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US04966967
出典データセットuspto-grants-1990_10
ORD IDord-b8b68b4a029d40cca1a79aeddaa89174
出典メモuspto-grants-1990_10