関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Butyl isocyanate | HCID 8110 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Potassium Hydroxide | HCID 14797 | — |
| 反応物 | 3-Trifluoromethyl-4'-hydroxy-alpha-ethylbenzhydrol | HCID 181876 | — |
| 溶媒 | Benzene | HCID 241 | — |
| 生成物 | 1-(3-Trifluoromethylphenyl)-1-(4-butylaminocarbonyloxyphenyl)-1-propanol | HCID 14727324 | — |
反応手順
8.9 g. of 3-trifluoromethyl-4'-hydroxy-α-ethyl-benzhydrol, 3.3 g. of n-butyl-isocyanate and 0.06 ml. of triethyl amine in 45 ml. of dry benzene are heated up to 50° C. under stirring, and the reaction mixture is kept at the same temperature for one additional hour. The progress of the reaction is monitored by thin layer chromatography. When the reaction is complete, the mixture is cooled to room temperature, the benzene solution is shaken with a 5% aqueous potassium hydroxide solution and washed to neutral with water. The organic phase is dried over anhydrous magnesium sulfate, filtered, and the solvent is distilled off under reduced pressure. The solid residue is crystallized from a mixture of ethyl acetate and n-hexane. 11.4 g. of the named compound are obtained, melting at 99° to 100° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04564630 |
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| 出典データセット | uspto-grants-1986_01 |
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| ORD ID | ord-f076cec6be3d4570b8a05b9fb53c40d8 |
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| 出典メモ | uspto-grants-1986_01 |
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