化工社化工社 化学情報印刷レポート · 研究参考用
Dichloromethane → 3-[3-[(Ethoxymethoxy)methyl]-1,2-benzisothiazol-5-yl]-1-methyl-6-(trifluoromethyl)-2,4(1H,3H)-pyrimidinedione
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dichloromethane | HCID 6344 | — |
| 反応物 | Chloromethyl ethyl ether | HCID 18523 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | 3-[3-(hydroxymethyl)-1,2-benzisothiazol-5-yl]-1-methyl-6-(trifluoromethyl)-2,4(1H,3H)-pyrimidinedione | HCID 22119821 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | 3-[3-[(Ethoxymethoxy)methyl]-1,2-benzisothiazol-5-yl]-1-methyl-6-(trifluoromethyl)-2,4(1H,3H)-pyrimidinedione | HCID 22119844 | — |
反応手順
To a mixture of 3-[3-(hydroxymethyl)-1,2-benzisothiazol-5-yl]-1-methyl-6-(trifluoromethyl)-2,4(1H,3H)-pyrimidinedione (0.800 g, 0.00224 mol) and methylene chloride is added ethyldiisopropylamine (0.780 ml, 0.00448 mol) followed by chloromethyl ethyl ether (0.310 ml, 0.00336 mol). The resultant mixture is stirred 42.5 hours at room temperature, diluted with ether, washed sequentially with 1 M aqueous hydrochloric acid, saturated sodium bicarbonate and brine, dried over anhydrous magnesium sulfate, filtered, and concentrated in vacuo to a yellow syrup. The syrup is chromatographed on silica gel with hexanes:ethyl acetate to give the product as a white 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 | US06156700 |
| 出典データセット | uspto-grants-2000_12 |
| ORD ID | ord-ddb3fbe77182416c926ff1265cfa9adf |
| 出典メモ | uspto-grants-2000_12 |