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HRID 277356作成日:2026年10月25日

Acetic Acid → 3-[3-(6-Methoxy-3,4-xylyl)-1,2-benzisothiazol-5-yl]-6-(trifluoromethyl)-2,4(1H,3H)-pyrimidinedione

https://huagongshe.com/reaction/277356

反応式

関与物質

役割名称HCID仕込み量
反応物Acetic AcidHCID 176—
反応物WaterHCID 962—
反応物2-(dimethylamino)-4-(trifluoromethyl)-6H-1,3-oxazin-6-oneHCID 3723862—
反応物5-Amino-3-(6-methoxy-3,4-xylyl)-1,2-benzisothiazoleHCID 18314503—
溶媒Diethyl EtherHCID 3283—
溶媒DichloromethaneHCID 6344—
生成物3-[3-(6-Methoxy-3,4-xylyl)-1,2-benzisothiazol-5-yl]-6-(trifluoromethyl)-2,4(1H,3H)-pyrimidinedioneHCID 1547761262.4%

反応手順

A mixture of 5-amino-3-(6-methoxy-3,4-xylyl)-1,2-benzisothiazole (8.53 g, 30.0 mmol), 2-dimethylamino-4-(trifluoromethyl)-6H-1,3-oxazin-6-one (6.87 g, 33.0 mmol) and acetic acid is refluxed for 2 hours, cooled, and poured into water. The resultant aqueous mixture is filtered to obtain a solid. A solution of the solid in methylene chloride is washed sequentially with water and brine, dried over anhydrous magnesium sulfate, and concentrated in vacuo to obtain an oil. Column chromatography of the oil using silica gel and a 5% diethyl ether in methylene chloride solution gives the title product as a yellow foam (8.37 g, 62.0%) which is identified by NMR spectral analyses.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US06355796B1
出典データセットuspto-grants-2002_03
ORD IDord-ffb87ddadc4547c0ae76559fff954cf8
出典メモuspto-grants-2002_03