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P-Toluenesulfonamide → 1,3-Dimethyl-5-tosyl-5,6-dihydro-4H-thieno[3,4-c]pyrrole
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | P-Toluenesulfonamide | HCID 6269 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 3,4-Bis(chloromethyl)-2,5-dimethylthiophene | HCID 288399 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 1,3-Dimethyl-5-tosyl-5,6-dihydro-4H-thieno[3,4-c]pyrrole | HCID 18947057 | 63.6% |
反応手順
A solution of 10 g (0.048 mol) of 3,4-bis(chloromethyl)-2,5-dimethylthiophene and 8.22 g of p-toluenesulphonamide in 600 ml of dry dimethylformamide is added dropwise, over 6 h, to a stirred suspension, heated to 100°-110° C., of 180 g of potassium carbonate in 900 ml of dimethylformamide. After the end of the addition, the mixture is maintained at the same temperature for 30 min, and then filtered. The solid is washed with dimethylformamide. The filtrate is concentrated under vacuum, and the residue is treated with 100 ml of ethanol, and filtered. The solid residue remaining is washed with ethanol and dried. 9.39 g of product are obtained. Melting point: 163°-164° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05380742 |
| 出典データセット | uspto-grants-1995_01 |
| ORD ID | ord-32ddc447f8a04f45a562d00df4e39c31 |
| 出典メモ | uspto-grants-1995_01 |