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Potassium Carbonate → 8-methyl-3,4-dihydro-2H-[1,3]thiazino[3,2-a]benzimidazole
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 1,3-Diiodopropane | HCID 12314 | — |
| 反応物 | HCID 178423448 | HCID 178423448 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 8-methyl-3,4-dihydro-2H-[1,3]thiazino[3,2-a]benzimidazole | HCID 66628146 | 25.3% |
反応手順
To a flask were added 2 g 2-mercapto-5-methylbenzimidazole, 4.2 g potassium carbonate, 4.0 g 1,3-diiodopropane and 60 ml N,N-dimethylformamide. The mixture was heated to 50 C under nitrogen for 5 hours and then cooled to 22 C. The reaction was quenched with 100 ml water and the product was extracted twice with ethyl acetate and washed twice with water. Following removal of the solvent, the product was recrystallized by dissolving in a hot mixture of 50 ml hexane with 10 ml 2-propanol. After cooling to 5 C, the product was filtered, washed with hexane and dried giving 0.63 g of an off-white solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07538931B2 |
| 出典データセット | uspto-grants-2009_05 |
| ORD ID | ord-9c57fcccb51746209a21e530f5334078 |
| 出典メモ | uspto-grants-2009_05 |