関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Acetate | HCID 517045 | — |
| 反応物 | tert-Butyl 4-oxopiperidine-1-carboxylate | HCID 735900 | — |
| 反応物 | N-Propylpiperazinium dibromide | HCID 3085288 | — |
| 反応物 | Sodium cyanoborohydride | HCID 5003444 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 4-(4-Propyl-piperazine-1-yl)-piperidine-1-carboxylic acid-tert-butylester | HCID 67163983 | 56% |
反応手順
42 g (0.50 mol) sodium acetate were added in portions to 73 g (0.25 mol) N-propylpiperazine dihydrobromide in 1 l methanol at 40° C. Subsequently, this was cooled to 0° C. and 50 g (0.25 mol) Boc-4-piperidon and 16 g (0.25 mol) sodium cyanoborohydride, in portions, were added, one after the other. Everything was then stirred at room temperature for 16 h. The reaction mixture was concentrated in a vacuum and then distributed between ethyl acetate and 1M NaOH. The organic phase was separated, washed with 1M NaOH, H2O and conc. NaCl solution, dried and concentrated in a vacuum. The residue was chromatographically purified over silica gel (mobile phase: MeOH/CH2Cl2=1/15). 43.6 g of the product were obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07951807B2 |
|---|
| 出典データセット | uspto-grants-2011_05 |
|---|
| ORD ID | ord-37a9e83a751c4ebd9bdbabc557cb2c63 |
|---|
| 出典メモ | uspto-grants-2011_05 |
|---|
