関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Toluene | HCID 1140 | — |
| 反応物 | Benzyl Chloride | HCID 7503 | — |
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | Methamphetamine | HCID 10836 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | Benzphetamine Hydrochloride | HCID 11558159 | 70% |
反応手順
To a 100 ml 3-neck flask fitted with a mechanical stirrer was added 17.10 g (0.1145 moles) of methamphetamine, 14.50 g (0.1368 mole) of sodium carbonate and 10.60 g of toluene. The reaction mass was heated to 120° C. and 16.18 g (0.1265 mole) of benzyl chloride was added over 180 minutes. The reaction was continued for a total of 6.75 hr. The reaction mass was cooled and transferred to a 500 ml flask equipped with a mechanical stirrer. To this flask was added 45 ml of toluene and 90 ml of water. The mixture was aggressively stirred to dissolve the salt. The layers were separated and the water layer was washed twice with 20 ml portions of toluene. The combined toluene layers were washed with 20 ml of water. Then to the stirred toluene layer was added 11.33 g of concentrated hydrochloric acid. The flask was equipped with a Dean-Stark trap and condenser and the water was removed by azeotropic distillation. There was 8.9 g of water recovered from the Dean-Stark trap. The organic material crystallized upon cooling between about 60° C. to about 40° C. affording 19.79 g of crude benzphetamine hydrochloride which is a 70% yield.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07750187B2 |
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| 出典データセット | uspto-grants-2010_07 |
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| ORD ID | ord-7202b0351b26437db630c823e82a8943 |
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| 出典メモ | uspto-grants-2010_07 |
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