化工社化工社 化学情報印刷レポート · 研究参考用
Sodium Cyanide → 4-Amino-1-t-butyl4-cyano-piperidine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Cyanide | HCID 8929 | — |
| 反応物 | Ammonium Chloride | HCID 25517 | — |
| 反応物 | 1-tert-Butyl-4-piperidone | HCID 73840 | — |
| 溶媒 | Ammonia | HCID 222 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 4-Amino-1-t-butyl4-cyano-piperidine | HCID 22063202 | — |
反応手順
1-t-Butyl-4-piperidone (1.3 g, 8.4 mmol, 1.0 equiv), NaCN (0.61 g, 12.6 mmol, 1.5 equiv), and NH4Cl (0.67 g, 12.6 mmol, 1.5 equiv) were combined in 34 mL of 2 M NH3 in MeOH. The mixture was refluxed for 2 h at which time an additional 34 mL of 2 M NH3 in MeOH was added followed by another 2 h at reflux. The mixture was cooled and filtered. The filtrate was concentrated in vacuo and the residue was triturated with CH2Cl2 and filtered again. The solution was concentrated to a thick red oil which was used without further purification; MS, m/z 182=M+1.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07279472B2 |
| 出典データセット | uspto-grants-2007_10 |
| ORD ID | ord-01e3e06a47054a8198aad7d0b833adf3 |
| 出典メモ | uspto-grants-2007_10 |