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Triethylamine → 3-Chloro-4-[4-(2-morpholin-4-yl-5-nitro-benzoyl)-piperazin-1-yl]-benzonitrile
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 2-Morpholin-4-yl-5-nitro-benzoyl chloride | HCID 17274153 | — |
| 反応物 | 3-Chloro-4-(piperazin-1-yl)benzonitrile | HCID 19367113 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 3-Chloro-4-[4-(2-morpholin-4-yl-5-nitro-benzoyl)-piperazin-1-yl]-benzonitrile | HCID 59793497 | — |
反応手順
A mixture of 40.6 mg (0.15 mmol) 2-Morpholin-4-yl-5-nitro-benzoyl chloride, 39.9 mg (0.18 mmol) 3-Chloro-4-piperazin-1-yl-benzonitrile (WO9625414) and 62.5 ul (0.45 mmol) NEt3 in 1 ml DCM was stirred at room temperature for 16 h. After evaporation of the volatiles the residue was taken up in 1 ml CH3CN/DMF/HCOOH 3/5/2 and subjected to preparative HPLC purification on reversed phase eluting with an acetonitrile/water gradient to yield after evaporation of the product fractions 4.9 mg (8%) of the title compound. MS (m/e): 456.2 (MH+, 100%)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07427612B2 |
| 出典データセット | uspto-grants-2008_09 |
| ORD ID | ord-d851dfe9333f4762bfe8c84bb68872c6 |
| 出典メモ | uspto-grants-2008_09 |