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Sulfuric Acid → 5-(2-Benzylaminopropoxy)salicylamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | Benzylamine | HCID 7504 | — |
| 反応物 | 5-(2-Oxopropoxy)salicylamide | HCID 13754333 | — |
| 反応物 | HCID 178418361 | HCID 178418361 | — |
| 触媒 | Platinum | HCID 23939 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 5-(2-Benzylaminopropoxy)salicylamide | HCID 13754334 | — |
反応手順
55 g of benzylamine and 1.25 g of conc. sulfuric acid are added to a solution of 104.5 g of 5-(2-oxo-propoxy)salicylamide in 1000 ml of methanol, and the mixture is hydrogenated, in the presence of 3.0 g of a Pt/C catalyst under normal conditions until 1 equivalent of hydrogen has been absorbed. The catalyst is filtered off, and the solution is then stirred up with about 10 g of pulverised calcium carbonate; the mixture is again filtered, and concentrated by evaporation. The oil remaining behind crystallises from isopropanol. Repeated recrystallisation from isopropanol yields 5-[2-(benzylamino)-propoxy]-salicylamide, m.p. 102°-104°.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04727067 |
| 出典データセット | uspto-grants-1988_02 |
| ORD ID | ord-fd0ebe5400be4198acdf81230619e204 |
| 出典メモ | uspto-grants-1988_02 |