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Sodium Hydroxide → 2-[2-(Dimethylamino)ethylthiomethyl]-5-methyl-2,3,6,7-tetrahydrofuro-[2,3-f]quinoline-7-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Captamine | HCID 25799 | — |
| 反応物 | 2-Bromomethyl-5-methyl-2,3,6,7-tetrahydrofuro[2,3-f]quinoline-7-one | HCID 23369645 | — |
| 溶媒 | Hydrochloric Acid | HCID 313 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 2-[2-(Dimethylamino)ethylthiomethyl]-5-methyl-2,3,6,7-tetrahydrofuro-[2,3-f]quinoline-7-one | HCID 23369673 | 91.1% |
反応手順
To a suspension of 2-bromomethyl-5-methyl-2,3,6,7-tetrahydrofuro-[2,3-f]quinoline-7-one (1. 765 g) in dimethylformamide (60 ml), hydrochloric acid salt of 2 (dimethylamino)ethylmercaptan (4.25 g) and caustic soda (2.40 g) in water (20 ml) were added and stirred at room temperature for 1 hour. The solvent was distilled off under reduced pressure. The residue was combined with water, and extracted with chloroform. The extract was washed with NaCl solution twice and dried and condensed. The residue was crystallized from chloroform--n-hexane to obtain 1.741 g of the title compound as white powder (mp.: 163°-165° C.).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05576324 |
| 出典データセット | uspto-grants-1996_11 |
| ORD ID | ord-9c5b9c9f1a514ec1a9a9042f54391201 |
| 出典メモ | uspto-grants-1996_11 |