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Triethylamine → trans-N-[2-(Dimethylamino)cyclohexyl]alpha,alpha,alpha-trifluoro-p-toluamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 4-(Trifluoromethyl)benzoyl chloride | HCID 67607 | — |
| 反応物 | N1,N1-dimethylcyclohexane-1,2-diamine | HCID 12447266 | — |
| 生成物 | trans-N-[2-(Dimethylamino)cyclohexyl]alpha,alpha,alpha-trifluoro-p-toluamide | HCID 53682390 | — |
反応手順
The titled amide was prepared according to general procedure B using p-trifluoromethyl-benzoyl chloride (4.17 g.; 0.02 mole), N,N-dimethylcyclohexane-1,2-diamine (2.84 g.; 0.02 mole) and triethylamine (2.02 g., 0.02 mole). The crude solid was crystallized from ether to give 4.766 g. (77% yield) of colorless needles, m.p. 141°-142°, raised to 141.5°-142.5° on recrystallization. uv λmax 222 nm (ε11,450), sh 245 (5,550); sh 260 (3,400); sh 276 (1.750), ir NH 3310; =CH 3030; N-alkyl 2770, 2740; C=O 1635; C=C 1575, 1510; amide II 1550; CF3 /ether 1330, 1190, 1165, 1130, 1105, 1065, 1020; aromatic 860; nmr in CDCl3 at 100 MHz was in accord. Mass spectrum M+ 314.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04152459 |
| 出典データセット | uspto-grants-1979_05 |
| ORD ID | ord-fdcd462a0c434e08a4bc313aa1f334ff |
| 出典メモ | uspto-grants-1979_05 |