참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | 3-Aminobenzonitrile | HCID 16702 | — |
| 반응물 | Bis(2-chloroethyl)amine hydrochloride | HCID 522769 | — |
| 용매 | O-Xylene | HCID 7237 | — |
| 용매 | Sodium Hydroxide | HCID 14798 | — |
| 생성물 | 1-(3-Cyanophenyl)piperazine | HCID 11480902 | 34% |
반응 단계
3-Aminobenzonitrile (6.1 g, 52 mmol) and bis(2-chloroethyl)amine hydrochloride (10 g, 57 mmol) were dissolved in xylene (100 ml), and the resulting solution was stirred at 150 to 160° C. for 5 hours. Supernatant fluid of the reaction solution was discarded, the remaining residue was dissolved in sodium hydroxide aqueous solution (1 N) and then the reaction product was extracted therefrom with ethyl acetate. The extract was washed with saturated brine, and then the compound obtained by the evaporation of the solvent under a reduced pressure was separated and purified by a silica gel column chromatography to obtain 3.2 g of the title compound (17 mmol, 34% in yield). A portion of the thus obtained compound was made into hydrochloric acid salt by treating it with hydrochloric acid-saturated methanol.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US06355642B1 |
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| 출처 데이터셋 | uspto-grants-2002_03 |
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| ORD ID | ord-16226fadb74f4ca2baebda3f682e8192 |
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| 출처 메모 | uspto-grants-2002_03 |
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