化工社化工社 化学情報印刷レポート · 研究参考用
4-Bromobenzaldehyde → Phenylmethyl (2S)-4-[(4-bromophenyl)methyl]-2-methyl-1-piperazine Carboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 4-Bromobenzaldehyde | HCID 70741 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | Sodium triacetoxyborohydride | HCID 5049666 | — |
| 反応物 | Benzyl (2S)-2-methylpiperazine-1-carboxylate | HCID 40425199 | — |
| 溶媒 | 1,2-Dichloroethane | HCID 11 | — |
| 生成物 | Phenylmethyl (2S)-4-[(4-bromophenyl)methyl]-2-methyl-1-piperazine Carboxylate | HCID 25224210 | 84.2% |
反応手順
A mixture of 4-bromobenzaldehyde (1.19 g, 6.42 mmol), phenylmethyl (2S)-2-methyl-1-piperazinecarboxylate (1.505 g, 6.42 mmol) and sodium triacetoxyborohydride (2.04 g, 9.63 mmol) in 1,2-DCE (15 ml) was stirred at room temperature overnight. Saturated aq. NaHCO3 solution was added and the mixture stirred for 30 mins. Product was extracted and the extracts dried (Na2SO4). Chromatography (0-30% EtOAc in pentane) gave the title compound (2.18 g). MS (ES): MH+ 403/405.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08536182B2 |
| 出典データセット | uspto-grants-2013_09 |
| ORD ID | ord-d3f1cc6cc426466f9662703f3e0ae627 |
| 出典メモ | uspto-grants-2013_09 |