참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Sodium Carbonate | HCID 10340 | — |
| 반응물 | 3-Chloro-1-propyne | HCID 12221 | — |
| 반응물 | TFMPP hydrochloride | HCID 3084246 | — |
| 용매 | Acetonitrile | HCID 6342 | — |
| 생성물 | N-(3-Trifluoromethyl-phenyl)-N'-propargyl-piperazine hydrochloride | HCID 13116712 | — |
반응 단계
3.2 g (0.012 mol) of N-(3-trifluoromethyl-phenyl)-piperazine hydrochloride, 0.9 g (0.012 mol) of propargyl chloride and 2.5 g (0.024 mol) of sodium carbonate were heated at 60° C. in 50 ml of absolute acetonitrile while stirring. Over a period of 15 hours, an additional 0.34 g (0.0046 mol) of propargyl chloride and 0.5 g (0.0046 mol) of sodium carbonate were added. The inorganic salts were removed by suction filtration, and the filtrate was evaporated under reduced pressure. The evaporation residue was dissolved in toluene, and the product solution was extracted with the calculated quantity of dilute hydrochloric acid. The aqueous phase was made alkaline with soda, and the base was extracted with ether. After drying with sodium sulfate, the organice phase was evaporated under reduced pressure, and the base was converted into its hydrochloride in conventional manner. White crystals from acetonitrile, melting point 218°-219° C. (decomposition). Yield: 2.7 g (73.8% of theory). The existence of these compounds was confirmed by elemental and spectrum analysis.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US04699910 |
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| 출처 데이터셋 | uspto-grants-1987_10 |
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| ORD ID | ord-d4343479822d4030b7c098531a0b7fe7 |
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| 출처 메모 | uspto-grants-1987_10 |
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