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Water → 2-Dimethylamino-2-Methyl-1-Propyl Tributylstannyl Ether
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | 2-(Dimethylamino)-2-methylpropanol | HCID 23435 | — |
| 反応物 | Bis(tributyltin) oxide | HCID 16682746 | — |
| 溶媒 | Benzene | HCID 241 | — |
| 生成物 | 2-Dimethylamino-2-Methyl-1-Propyl Tributylstannyl Ether | HCID 22757038 | — |
反応手順
2-Dimethylamino-2-Methyl-1-Propyl Tributylstannyl Ether is prepared from 59.6 gm (0.1 mole) bis(tributyltin) oxide and 23.4 gm (0.2 mole) 2-dimethylamino-2-methyl-1-propanol in 200 ml benzene. This is stirred and heated to reflux in a system that contains a Dean-Starke tube. After 30 minutes water began to collect in the Dean-Starke tube and after 46 hours only 1.6 ml of water (theory 1.8 ml) had collected. Solvent is stripped off on a rotating evaporator to provide 78.3 gm of straw colored liquid. This is fractionated at reduced pressure to collect the desired product, 52.7 gm of water-white liquid (Percent yield - 65), at 132°-137° C. at 0.5 mm. Infrared spectral analysis shows this to be the desired ether.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04128429 |
| 出典データセット | uspto-grants-1978_12 |
| ORD ID | ord-1196f53696f64bde99386c13c8232522 |
| 出典メモ | uspto-grants-1978_12 |