関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Acetic Acid | HCID 176 | — |
| 反応物 | 4-Ethoxybenzaldehyde | HCID 24834 | — |
| 反応物 | Sodium cyanoborohydride | HCID 5003444 | — |
| 反応物 | 4-[{N-(2-amino5-chlorobenzoyl)glycyl}aminomethyl]piperidine | HCID 18426216 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 4-[{N-(2-amino-5-chlorobenzoyl)glycyl}aminomethyl]-1-(4-ethoxybenzyl)piperidine | HCID 18426129 | — |
反応手順
Sodium cyanoborohydride (140 mmol) in methanol (0.4 mL) was added to a mixture of 4-[(N-(2-amino-5-chlorobenzoyl)glycyl)aminomethyl]piperidine (0.10 mmol), 4-ethoxybenzaldehyde (0.10 mmol), acetic acid (0.050 mL), and methanol (1.6 mL). The reaction mixture was stirred at 60° C. for 14 h. The reaction mixture was loaded onto Varian™ SCX column and washed with CH3OH (20 mL). Product was eluted using 2 N NH3 in CH3OH (6 mL) and concentrated. Preparative TLC (SiO2, AcOEt/CH3OH 5:1) afforded 4-[{N-(2-amino-5-chlorobenzoyl)glycyl}aminomethyl]-1-(4-ethoxybenzyl)piperidine (Compound No. 1429) and 1-(4-ethoxybenzyl)-4-[{N-(2-(4-ethoxybenzyl)amino-5-chlorobenzoyl)glycyl)aminomethyl]piperidine (Compound No. 1433).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US06362177B1 |
|---|
| 出典データセット | uspto-grants-2002_03 |
|---|
| ORD ID | ord-240e1e92bcba4ddd8befbfad2c8266a9 |
|---|
| 出典メモ | uspto-grants-2002_03 |
|---|
