関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 5,6,7,8-Tetrahydroisoquinoline | HCID 119010 | — |
| 反応物 | 2-Methanesulfonyloxyethyl disulfide | HCID 23117209 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | HCID 86630319 | HCID 86630319 | — |
反応手順
3.2 g of 5,6,7,8-tetrahydroisoquinoline and 0.7 g of potassium carbonate were mixed in 3 ml of acetonitrile and brought to 80° C. A solution of 3.4 g of disulfanediyldiethane-2,1-diyl dimethane sulfonate in 3 ml of acetonitrile was added in 10 min. Stirring was maintained for 8 h at 80° C. and then the reaction medium was brought back to ambient temperature, filtered, and concentrated under vacuum. 6 ml of dichloromethane were added and the solution was poured dropwise into 500 ml of ethyl ether. The oil that had been separated by settling out was reprocessed twice by diluting in 6 ml of methanol and adding to 500 ml of ethyl ether, and a final time by diluting in 6 ml of dichloromethane and adding to 500 ml of ethyl ether. After drying under vacuum, 5.2 g of brown solid were recovered. The analyses were in compliance with the expected structure.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07744657B2 |
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| 出典データセット | uspto-grants-2010_06 |
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| ORD ID | ord-cd1ca81fc66c4efbb1f88f5beb425df2 |
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| 出典メモ | uspto-grants-2010_06 |
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