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Ammonia → 2-Amino-5-methylbenzamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ammonia | HCID 222 | — |
| 反応物 | Tetrahydrofuran | HCID 8028 | — |
| 反応物 | 2-Amino-5-methylbenzoic acid | HCID 76255 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 2-Amino-5-methylbenzamide | HCID 10329436 | — |
反応手順
A mixture of 15 g of 2-amino-5-methylbenzoic acid, 16 g of 1,1-carbonyldiimidazole and 500 ml of tetrahydrofuran was stirred for 2 hours at room temperature and then saturated with anhydrous ammonia with ice bath cooling. After 24 hours, 50 ml of water was added and the mixture was concentrated under reduced pressure to a solid residue. This solid Was partially dissolved in 500 ml of dichloromethane and then washed with 200 ml of 0.1 N sodium hydroxide and 200 ml of water. The dichloromethane solution was dried and concentrated to a solid Which Was crystallized from ethyl acetate/hexane, giving 3.0 g of 2-amino-5-methylbenzamide as straw-colored crystals, mp 171°-174° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05001157 |
| 出典データセット | uspto-grants-1991_03 |
| ORD ID | ord-e68c99d67c3e4389bcd7777e33b88a9f |
| 出典メモ | uspto-grants-1991_03 |