참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Acetonitrile | HCID 6342 | — |
| 반응물 | 2-Methylpyridine | HCID 7975 | — |
| 반응물 | N-methyl-2-pyrrolidone | HCID 13387 | — |
| 반응물 | Disulfide, bis(2-bromoethyl) | HCID 572268 | — |
| 생성물 | 1,1'-(Disulphanediyldiethane-2,1-diyl)bis(2-methylpyridinium)dibromide | HCID 86630321 | — |
반응 단계
A mixture of 56 g of 1-bromo-2-[(2-bromoethyl)-disulphanyl]ethane and 15 ml of N-methylpyrrolidone (NMP) is poured dropwise onto 35 g of 2-picoline with stirring, at 80° C. The mixture (white suspension) is kept stirring at 80° C. for 30 min, 100 ml of ACN are added, and the stirring is maintained at 80° C. for 90 min. After cooling, the solid obtained is filtered off, washed with 100 ml of ACN and then dried. 56.2 g of brown powder are recovered. 45 g of this powder are suspended in 300 ml of iPrOH, at reflux. Once the temperature has dropped to 40° C., the solid is filtered off, washed with 3 times 100 ml of iPrOH and dried under vacuum. 40.56 g of a light beige product are obtained. The analyses are in conformity with the expected structure.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08038732B2 |
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| 출처 데이터셋 | uspto-grants-2011_10 |
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| ORD ID | ord-c909be4925074e71b829f2562945a11d |
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| 출처 메모 | uspto-grants-2011_10 |
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