関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hexanoic Acid | HCID 8892 | — |
| 反応物 | Dicyclohexylcarbodiimide | HCID 10868 | — |
| 反応物 | 4-Pyrrolidinopyridine | HCID 75567 | — |
| 反応物 | 4-{2-(4-Hexylphenyl)thiazole-5-yl}phenol | HCID 23354762 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 2-(4-Hexylphenyl)-5-(4-hexanoyloxyphenyl)thiazole | HCID 23354788 | 70.1% |
反応手順
In a 200 ml-round-bottomed flask, 2.00 g (5.93 mM) of 2-(4-hexylphenyl)-5-(4-hydroxyphenyl)thiazole, 0.76 g (6.54 mM) of hexanoic acid and 40 ml of dichloromethane were placed and mixed. To the solution, 1.24 g (6.01 mM) of N,N'-dicyclohexylcarbodiimide and 0.10 g of 4-pyrrolidinopyridine were successively added under stirring at room temperature, followed by further stirring for 7 hours at room temperature to precipitate N,N'-dicyclohexylurea. The resultant N,N'-dicyclohexylurea was filtered off and the solvent of the filtrate was distilled-off under reduced pressure. The residue was purified by silica gel column chromatography (eluent: toluene/ethyl acetate=100/1) and recrystallized from a mixture solvent of toluene-methanol to obtain 1.81 g of 2-(4-hexylphenyl)-5-(4-hexanoyloxyphenyl)thiazole (Yield: 70.1%). ##STR198##
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05595685 |
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| 出典データセット | uspto-grants-1997_01 |
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| ORD ID | ord-6ae0a5b6cb574530aaa67cc74c1ee629 |
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| 出典メモ | uspto-grants-1997_01 |
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