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Dichloromethane → 2-(2-methoxyphenethyl)imino-N-(ethylthiocarbamoyl)-5,5-dimethyl-1,3-thiazine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dichloromethane | HCID 6344 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | O-ethyl chloromethanethioate | HCID 5325481 | — |
| 反応物 | 2-(2-Methoxyphenethyl)imino-5,5-dimethyl-1,3-thiazine | HCID 22639987 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 2-(2-methoxyphenethyl)imino-N-(ethylthiocarbamoyl)-5,5-dimethyl-1,3-thiazine | HCID 22639982 | 60% |
反応手順
To a mixture of 2-(2-methoxyphenethyl)imino-5,5-dimethyl-1,3-thiazine (0.28 g), triethylamine (0.15 g) and dichloromethane (5 ml) was added dropwise for 3 minutes ethyl chlorothiocarbonate (0.15 g). The mixture was stirred at room temperature for 2 hours. To the solution was added water (30 ml). The mixture was extracted with diethylether (60 ml), dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The obtained residue was purified by silica gel column chromatography (n-hexane/ethyl acetate) to give 2-(2-methoxyphenethyl)imino-N-(ethylthiocarbamoyl)-5,5-dimethyl-1,3-thiazine (0.21 g, yield: 60%) as colorless oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07420053B2 |
| 出典データセット | uspto-grants-2008_09 |
| ORD ID | ord-05f6df7952f2492ca9ddec50276d3ca1 |
| 出典メモ | uspto-grants-2008_09 |