関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Acetonitrile | HCID 6342 | — |
| 反応物 | 2-Methylpyridine | HCID 7975 | — |
| 反応物 | N-methyl-2-pyrrolidone | HCID 13387 | — |
| 反応物 | Disulfide, bis(2-bromoethyl) | HCID 572268 | — |
| 生成物 | 1,1'-(Disulphanediyldiethane-2,1-diyl)bis(2-methylpyridinium)dibromide | HCID 86630321 | — |
反応手順
A mixture of 56 g of 1-bromo-2-[(2-bromoethyl)disulfanyl]ethane and 15 ml of N-methylpyrrolidone (NMP) was poured dropwise over 35 g of 2-picoline with stirring at 80° C. The mixture (white suspension) continued to be stirred for 30 min at 80° C., then 100 ml of acetonitrile were added and the stirring was continued at 80° C. for 90 min. After cooling, the solid obtained was filtered, washed with 100 ml of acetonitrile, then dried. 56.2 g of brown powder were recovered. 45 g of this powder were suspended in 300 ml of isopropanol, under reflux. Once the temperature dropped to 40° C., the solid was filtered, washed with three times 100 ml of isopropanol and dried under vacuum. Thus, 40.56 g of a light beige product was obtained. Analyses were in accordance with the expected structure.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08097044B2 |
|---|
| 出典データセット | uspto-grants-2012_01 |
|---|
| ORD ID | ord-be580d6107a34e46ace26a1080ca1113 |
|---|
| 出典メモ | uspto-grants-2012_01 |
|---|