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1-((Pyridin-4-yl)methyl)piperazine → 1-({3-[2-(2,4-Dichlorophenyl)ethoxy]-4-methoxyphenyl}carbonyl)-4-(pyridin-4-ylmethyl)piperazine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1-((Pyridin-4-yl)methyl)piperazine | HCID 808715 | — |
| 反応物 | O-[(Ethoxycarbonyl)cyanomethylenamino]-N,N,N',N'-tetramethyluronium tetrafluoroborate | HCID 2733286 | — |
| 反応物 | 3-[2-(2,4-Dichlorophenyl)ethoxy]-4-methoxybenzoic acid | HCID 15480332 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 1-({3-[2-(2,4-Dichlorophenyl)ethoxy]-4-methoxyphenyl}carbonyl)-4-(pyridin-4-ylmethyl)piperazine | HCID 10185372 | — |
反応手順
0.100 g (0.29 mmol) of 3-[2-(2,4-Dichloro-phenyl)-ethoxy]-4-methoxy-benzoic acid was dissolved in 2 ml of DMF and treated with 0.146 ml (1.16 mmol) of N-NEM and 51 mg (0.29 mmol) of 1-Pyridin-4-ylmethyl-piperazine and 0.098 g (0.3 mmol) of TOTU. The solution was stirred for 1 h at RT. The solvent was removed under reduced pressure, the residue was taken-up in DCM and the solution was washed three times with saturated aqueous sodium bicarbonate. The organic phase was dried with sodium sulphate, filtered and the solvent was removed under reduced pressure. The residue was chromatographed on silica gel eluting with n-heptane/ethyl acetate (1/1), ethyl acetate, and ethyl acetate/MeOH (10/1).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06953857B2 |
| 出典データセット | uspto-grants-2005_10 |
| ORD ID | ord-4c76c119dd8d472b9c165ee6df40de5b |
| 出典メモ | uspto-grants-2005_10 |