関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | N,N-Diethylethylenediamine | HCID 60993 | — |
| 反応物 | 1,1'-Carbonyldiimidazole | HCID 68263 | — |
| 反応物 | N-(1-methylethyl)-4-(phenylsulfonyl]-1-butylamine | HCID 13655072 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | N'-[2-(Diethylamino)ethyl]-N-(1-methylethyl)-N-[4-(phenylsulfonyl)butyl]urea hydrate | HCID 20152850 | 69.8% |
反応手順
A solution of 1,1'-carbonyldiimidazole (6.00 g, 0.037 mole) and N,N-diethylethylenediamine (4.00 g, 0.034 mole) was stirred at room temperature for 2 hours in 200 ml of tetrahydrofuran. A solution of N-(1-methylethyl)-4-(phenylsulfonyl]-1-butylamine (free base 7.99 g, 0.0313 mole) in 100 ml of tetrahydrofuran was added and the solution was heated overnight at reflux. The reaction was stripped to dryness and the residue dissolved in chloroform. The chloroform was extracted with water, dried (sodium sulfate), filtered, and removed in vacuo. A dark brown oil was obtained upon removal of chloroform. This oil was subjected to flash chromatography on Silica Gel using 0.1N ammonium hydroxide-methanol for elution. This chromatography furnished 5.37 g (42.2% yield) of clear oil after drying in vacuo 18 hours at 60° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04724235 |
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| 出典データセット | uspto-grants-1988_02 |
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| ORD ID | ord-f4da05c15f66425caadd5d8639eb6bb2 |
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| 出典メモ | uspto-grants-1988_02 |
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