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Benzyltrimethylammonium hydroxide → 2-[2-(Pyridin-4-yl)propyl]-1lambda~6~,2-thiazolidine-1,1-dione
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Benzyltrimethylammonium hydroxide | HCID 66854 | — |
| 反応物 | Pyridine, 4-(1-methylethenyl) | HCID 529351 | — |
| 反応物 | 1,3-Propanesultam | HCID 642157 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 生成物 | 2-[2-(Pyridin-4-yl)propyl]-1lambda~6~,2-thiazolidine-1,1-dione | HCID 20434938 | — |
反応手順
A mixture of 4-isopropenyl pyridine (1.79 g) and isothiazolidine-1,1-dioxide (1.81 g) was heated at 130° C. during the addition of "Triton B" (Trade Mark, trimethylbenzylammonium hydroxide) (0.25 g added every hour for four hours; 40% solution in water). After stirring for 16 hours at 130° the mixture was cooled and taken in chloroform (50 cm3) and water (50 cm3). The aqueous phase was extracted with chloroform (3×20 cm3) and the dried (MgSO4) extracts were evaporated to given an oil. Chromatography on silica ("Merck 60. 9385") eluting with ethyl acetate gave 2-[2-(4-pyridyl)prop-1-yl]isothiazolidine-1,1-dioxide which crystallised from ethyl acetate-hexane as needles, m.p. 90°-92° (1.01 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04489075 |
| 出典データセット | uspto-grants-1984_12 |
| ORD ID | ord-7058774eda464732bce4cd4405a853c3 |
| 出典メモ | uspto-grants-1984_12 |