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2-(dimethylamino)-4-(trifluoromethyl)-6H-1,3-oxazin-6-one → Ethyl 5-[3,6-dihydro-2,6-dioxo-4-(trifluoromethyl)-1(2H)-pyrimidinyl]-1,2-benzisothiazole-3-acetate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2-(dimethylamino)-4-(trifluoromethyl)-6H-1,3-oxazin-6-one | HCID 3723862 | — |
| 反応物 | Ethyl 5-amino-1,2-benzisothiazole-3-acetate | HCID 11770464 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | Ethyl 5-[3,6-dihydro-2,6-dioxo-4-(trifluoromethyl)-1(2H)-pyrimidinyl]-1,2-benzisothiazole-3-acetate | HCID 10960337 | — |
反応手順
A mixture of ethyl 5-amino-1,2-benzisothiazole-3-acetate (0.748 g, 3.16 mmol) and 2-dimethylamino-4-(trifluoromethyl)-6H-1,3-oxazin-6-one (0.660 g, 3.17 mmol) in acetic acid is refluxed for three hours, concentrated in vacuo, and diluted with saturated sodium hydrogen carbonate solution. The resultant mixture is extracted with methylene chloride. The combined organic extracts are washed with water, dried over anhydrous sodium sulfate, and concentrated in vacuo to give the title product as a tan solid which is identified by NMR spectral analysis.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06355796B1 |
| 出典データセット | uspto-grants-2002_03 |
| ORD ID | ord-ffa3f6e12c80420e92e029f0313609f4 |
| 出典メモ | uspto-grants-2002_03 |