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Dichloromethane → 4-[[3-(p-Chlorophenyl)propyl]methylamino]benzoic acid, ethyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dichloromethane | HCID 6344 | — |
| 反応物 | Methanesulfonyl Fluoride | HCID 11207 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Ethyl 4-{[3-(4-chlorophenyl)propyl]amino}benzoate | HCID 13079692 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 4-[[3-(p-Chlorophenyl)propyl]methylamino]benzoic acid, ethyl ester | HCID 44278887 | — |
反応手順
A mixture of 1.0 g. of ethyl 4-[3-(p-chlorophenyl)propylamino]benzoate, 20 ml. of dry dichloromethane and 2.5 ml. of methane sulfonyl fluoride is stirred for 18 hours, then refluxed for 3 hours. The solution is poured into 30 ml. of water and adjusted to pH 10 with 10N sodium hydroxide. The dichloromethane layer is separated and saved. The aqueous layer is extracted with two 20 ml. portions of dichloromethane. The organic layers are combined, washed with 10 ml. of water, dried over anhydrous magnesium sulfate, and evaporated to yield 1.80 g. of the desired product as a light yellow oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04489094 |
| 出典データセット | uspto-grants-1984_12 |
| ORD ID | ord-fece9dcecc9d4259b9318987b022f9b8 |
| 出典メモ | uspto-grants-1984_12 |