関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 1,2-Ethanediamine, N2-[2-(diethylamino)ethyl]-N1,N1-diethyl- | HCID 67154 | — |
| 反応物 | N-(1-methylethyl)-N-[2-(phenylsulfonyl)ethyl]carbamic chloride | HCID 13655164 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | N,N-Bis[2-(diethylamino)ethyl]-N'-(1-methylethyl)-N'-[2-(phenylsulfonyl)ethyl]urea | HCID 14855301 | — |
反応手順
A mixture of 7.67 g (0.0265 mole) of N-(1-methylethyl)-N-[2-(phenylsulfonyl)ethyl]carbamic chloride and 6.24 g (0.029 mole) of N'-[2-(diethylamino)ethyl]-N,N-diethyl-1,2-ethanediamine and 2.73 g (0.0270 mole) of triethylamine in 400 ml of tetrahydrofuran was refluxed for 6 hr and then was stirred at room temperature for 7 hr. The solvent was removed in vacuo and the residue was partitioned between methylene chloride and dilute sodium hydroxide. The methylene chloride solution was dried over sodium sulfate, and the solvent was removed in vacuo to give an oil. This was dissolved in ether, and the solution was extracted with three portions of water. The ether solution was dried over sodium sulfate, and the solvent was removed in vacuo to give an oil. This was pumped under high vacuum at 56° C. for 20 hr to give the title compound as an oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04895840 |
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| 出典データセット | uspto-grants-1990_01 |
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| ORD ID | ord-279c13ebf324458dab675d5378c01dc5 |
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| 出典メモ | uspto-grants-1990_01 |
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