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Diisopropylethylamine → 4-tert-Butoxycarbonyl-1-[(6-chloronaphthalen-2-yl)sulfonyl]-2-ethoxycarbonylpiperazine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | 6-Chloronaphthalene-2-sulfonyl chloride | HCID 10635129 | — |
| 反応物 | 1-tert-Butyl 3-ethyl piperazine-1,3-dicarboxylate | HCID 11402671 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 4-tert-Butoxycarbonyl-1-[(6-chloronaphthalen-2-yl)sulfonyl]-2-ethoxycarbonylpiperazine | HCID 69700224 | — |
反応手順
In dichloromethane (18 ml), 1-tert-butoxycarbonyl-3-ethoxycarbonylpiperazine (517 mg) and 6-chloro-2-naphthylsulfonyl chloride (588 mg) were dissolved under ice cooling. To the resulting solution, diisopropylethylamine (0.59 ml) was added, followed by stirring at room temperature for 63 hours. The residue obtained by distilling off the solvent under reduced pressure was purified by chromatography on a silica gel column (hexane:ethyl acetate=3:1), whereby the title compound (688 mg, 71%) was obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06747023B1 |
| 出典データセット | uspto-grants-2004_06 |
| ORD ID | ord-49e9655c06184cefb9e063ca7e5b7913 |
| 出典メモ | uspto-grants-2004_06 |