関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hexane | HCID 8058 | — |
| 反応物 | 2-Chlorobenzylamine | HCID 66648 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | 2-(2-Bromoethyl)-3-(bromomethyl)thiophene | HCID 69311722 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | Ticlopidine | HCID 5472 | 78% |
反応手順
At below 5° C., 5.0 g of 2-(2-bromoethyl)-3-bromomethylthiophene obtained in Example 7 was dissolved in 50 mL of acetonitrile, and added thereto was a solution obtained by dissolving 2.7 g of 2-chlorobenzylamine and 6.8 g of diisopropylethylamine in 25 mL of acetonitrile. The resulting mixture was refluxed for 5 hours, and concentrated by evaporation under reduced pressure. The residue was dissolved in 100 mL of ethyl acetate, and washed twice with 70 mL portions of water. The organic layer was washed with 50 mL of saturated sodium chloride aqueous solution and concentrated under reduced pressure. The dark yellow colored oily residue thus obtained was subjected to a silica gel column chromatography (eluent, n-hexane:ethyl acetate=5:1) to obtain 3.6 g (yield of 78%) of the title compound as a yellowish oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07449580B2 |
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| 出典データセット | uspto-grants-2008_11 |
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| ORD ID | ord-3dbc198f823c4ccca4c7a84853069b93 |
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| 出典メモ | uspto-grants-2008_11 |
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