참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Toluene | HCID 1140 | — |
| 반응물 | Benzyl Chloride | HCID 7503 | — |
| 반응물 | Sodium Carbonate | HCID 10340 | — |
| 반응물 | Methamphetamine | HCID 10836 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | Benzphetamine Hydrochloride | HCID 11558159 | 70% |
반응 단계
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.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07750187B2 |
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| 출처 데이터셋 | uspto-grants-2010_07 |
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| ORD ID | ord-7202b0351b26437db630c823e82a8943 |
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| 출처 메모 | uspto-grants-2010_07 |
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