関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1,4-Dioxane | HCID 31275 | — |
| 反応物 | Ethyl 2-((propan-2-yl)amino)acetate | HCID 351625 | — |
| 反応物 | Phenyl N-(4-(4-(4-methoxyphenyl)piperazin-1-yl)phenyl)carbamate | HCID 981607 | — |
| 触媒 | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | HCID 14152935 | HCID 14152935 | 73% |
反応手順
A mixture of 5 parts of phenyl[4-[4-(4-methoxyphenyl)-1-piperazinyl]phenyl]carbamate, 3 parts of ethyl[(1-methylethyl)amino]acetate, 1 part of N,N-dimethyl-4-pyridinamine and 100 parts of 1,4-dioxane was stirred and refluxed overnight. The warm solution was saturated with water and allowed to cool. The solution was poured onto water and extracted with trichloromethane. The extract was washed with water, dried, filtered and evaporated. The residue was purified by filtration over silica gel using a mixture of trichloromethane and methanol (98:2 by volume) as eluent. The filtrate was evaporated and the residue was crystallized from methylbenzene, yielding 3.7 parts (73%) of 3-[4-[4-(4-methoxyphenyl)-1-piperazinyl]phenyl]-1-(1-methylethyl)-2,4-imidazolidinedione; mp. 193.7° C. (38).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04735942 |
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| 出典データセット | uspto-grants-1988_04 |
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| ORD ID | ord-be92ae4a412444b888a6a9a14e4eb534 |
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| 出典メモ | uspto-grants-1988_04 |
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