참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Acetonitrile | HCID 6342 | — |
| 반응물 | 4-Methylpyridine | HCID 7963 | — |
| 반응물 | N-methyl-2-pyrrolidone | HCID 13387 | — |
| 반응물 | Disulfide, bis(2-bromoethyl) | HCID 572268 | — |
| 생성물 | 1,1'-(Disulphanediyldiethane-2,1-diyl)bis(4-methylpyridinium)dibromide | HCID 86630322 | 90% |
반응 단계
67 g of 4-picoline were diluted in 100 ml of acetonitrile and the mixture was brought to 80° C. A mixture of 60 g of 1-bromo-2-[(2-bromoethyl)disulphanyl]ethane and 15 ml of N-methylpyrrolidone (NMP) was added over 5 min. After stirring for 4 h at 85° C., the mixture was cooled. The solid obtained was filtered, rinsed with 3×200 ml of acetonitrile then dissolved in 800 ml of isopropanol (under reflux). After cooling, 1 l of ethyl ether was added. The precipitate formed was filtered, rinsed with 3×200 ml of ethyl ether, then dried. The off-white powder obtained (73.77 g) very predominantly contained (>90%) the expected product which was used as such for the following step.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08097044B2 |
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| 출처 데이터셋 | uspto-grants-2012_01 |
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| ORD ID | ord-2721f4de1b234b248592a9f78d769c1a |
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| 출처 메모 | uspto-grants-2012_01 |
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