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Oxalic Acid → 3-(4-Trifluoromethylphenoxy)-N-methyl-1-azetidinecarboxamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Oxalic Acid | HCID 971 | — |
| 反応物 | Methyl Isocyanate | HCID 12228 | — |
| 反応物 | Potassium Hydroxide | HCID 14797 | — |
| 反応物 | 3-[4-(Trifluoromethyl)phenoxy]azetidine | HCID 12812499 | — |
| 溶媒 | Benzene | HCID 241 | — |
| 生成物 | 3-(4-Trifluoromethylphenoxy)-N-methyl-1-azetidinecarboxamide | HCID 13420166 | — |
反応手順
The oxalic acid salt of 3-(4-trifluoromethylphenoxy) azetidine (13.0 g., 0.042 mole) was partitioned between 50 ml. of benzene and 50 ml. of potassium hydroxide solution. The benzene layer was dried over calcium sulfate and filtered, and to the stirring dried benzene solution was added 2.6 g. (0.046 mole) of methyl-isocyanate. Stirring was continued overnight. The mixture was concentrated at reduced pressure and the solid residue was recrystallized from a mixture of isopropyl ether-ethyl acetate. The product weighed 7.5 g. (65%) and melted at 154°-157° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04226861 |
| 出典データセット | uspto-grants-1980_10 |
| ORD ID | ord-05ba8cda715a4cb3864f6eec80ea4e74 |
| 出典メモ | uspto-grants-1980_10 |