Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
HRID 621512생성일: 2026년 10월 27일
Potassium Carbonate → 1-(4-Hydroxyphenyl)-4-(3-cyano-4-methyl-6-phenylpyrid-2-yl)piperazine
https://huagongshe.com/reaction/621512
참여 물질
| 역할 | 이름 | HCID | 투입량 |
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| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | 2-Chloro-4-methyl-6-phenylnicotinonitrile | HCID 833688 | — |
| 반응물 | p-(1-Piperazinyl)phenol dihydrobromide | HCID 2723591 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | 1-(4-Hydroxyphenyl)-4-(3-cyano-4-methyl-6-phenylpyrid-2-yl)piperazine | HCID 14074118 | 51.1% |
반응 단계
12.26 g (36 mmol) of 1-(4-hydroxyphenyl)piperazine dihydrobromide, 8.24 g (36.1 mmol) of 2-chloro-3-cyano-4-methyl-6-phenylpyridine and 7.46 g (54 mmol) of powdered K2CO3 in 135 ml of absolute DMF were reacted at 90° C. according to the procedure described in Example 20. The mixture was subsequently stirred for 10 hours at 110° C. After removal of the DMF by distillation, the residue was taken up in CH2Cl2 /water. After thorough mixing, separating the phases and extraction of the aqueous solution, the CH2Cl2 extracts were combined, dried and evaporated. The crystalline residue (14.6 g) was recrystallized three times as follows. The substance was dissolved in a boiling mixture of CH2Cl2 /CH3OH 1:1, and the majority of the CH2Cl2 was then removed by distillation. A product crystallized out of the CH3OH solution obtained, and was filtered off under suction and again recrystallized in this fashion. Further impure substance was isolated from the mother liquors by concentration etc, and this was finally recrystallized again as described above. In this fashion, 6.82 g (=51% yield) of 1-(4-hydroxyphenyl)-4-(3-cyano-4-methyl-6-phenylpyrid-2-yl)piperazine, melting point 207°-08° C., were obtained;
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US04824846 |
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| 출처 데이터셋 | uspto-grants-1989_04 |
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| ORD ID | ord-03f23008a32843ecb952b831ce8d8401 |
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| 출처 메모 | uspto-grants-1989_04 |
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