関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Potassium Hydroxide | HCID 14797 | — |
| 反応物 | 4-Iodobenzyl bromide | HCID 954258 | — |
| 反応物 | 2-Butyl-1,3-diazaspiro[4.4]non-1-en-4-one | HCID 10176511 | — |
| 触媒 | Tetrabutylammonium hydrogen sulfate | HCID 94433 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 2-Butyl-3-(4-iodobenzyl)-1,3-diazaspiro[4.4]non-1-en-4-one | HCID 11996426 | 88% |
反応手順
A solution of 23.07 g (100 mmol) of the hydrochloride of 2-butyl-1,3-diazaspiro[4,4]non-1-en-4-one and 19.8 g of potassium hydroxide in 100 mL de water is added to a solution of 29.7 g (100 mmol) of 4-iodobenzyl bromide and 3.4 g (10 mmol) of tetrabutylammonium bisulphate in 30 mL of toluene, and the mixture is heated at reflux for 1 hr. After cooling to 25° C., 100 mL of water is added and the phases are separated. To the organic phase is added 10 mL of concentrated hydrochloric acid, 100 mL is evaporated at reduced pressure, 300 mL of ethyl acetate is added and the resulting solid is filtered to give 39.6 g (88%) of the title compound in the form of hydrochloride.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07741492B2 |
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| 出典データセット | uspto-grants-2010_06 |
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| ORD ID | ord-cfa93898b13c4cddbdf0bab68e95b661 |
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| 出典メモ | uspto-grants-2010_06 |
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