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Sodium Hydroxide → 3-Phenyl-3-(2,4,6-trichlorobenzenesulphonamido)propionic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | DL-beta-Phenylalanine | HCID 69189 | — |
| 反応物 | 2,4,6-Trichlorobenzenesulfonyl chloride | HCID 521335 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | 3-Phenyl-3-(2,4,6-trichlorobenzenesulphonamido)propionic acid | HCID 23002624 | 73.5% |
反応手順
1.15 g of 3-amino-3-phenylpropionic acid are dissolved in 25 ml of dioxane and 7 ml of 1N sodium hydroxide and 1.95 g of 2,4,6-trichlorobenzenesulphonyl chloride in 5 ml of dioxane are gradually added, while maintaining the pH at 10.5-11 by addition of 1N sodium hydroxide. After stirring for 2 hours at RT, the mixture is diluted with 100 ml of water, extracted twice with EtOAc and acidified to pH=2 by addition of 6N HCl. The solid formed is drained, washed with water and dried at 40° C. 2.09 g of the expected product are obtained, m.p.−218-219° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06610882B2 |
| 出典データセット | uspto-grants-2003_08 |
| ORD ID | ord-4802316e568349b6a8b39cfad6d851d1 |
| 出典メモ | uspto-grants-2003_08 |