化工社化工社 化学情報印刷レポート · 研究参考用
Hydrogen Peroxide → 2,3-Diaza-spiro[4.5]dec-2-ene
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrogen Peroxide | HCID 784 | — |
| 反応物 | [1-(Aminomethyl)cyclohexyl]methanamine | HCID 71994 | — |
| 反応物 | Sodium Hypochlorite | HCID 23665760 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 2,3-Diaza-spiro[4.5]dec-2-ene | HCID 59339453 | — |
反応手順
C-(1-Aminomethyl-cyclohexyl)-methylamine (10.0 g) was taken up in a mixture of H2O (40 mL) and MeOH (10 mL), and cooled in an ice bath. Simultaneously, H2O2 (44.3 mL of a 30% solution, 6 equiv.) and NaClO (125.5 mL of a 10% solution, 2.4 equiv.) were added dropwise, the ice bath was removed, and the mixture was stirred for 45 min. at room temperature. Extraction with DCM, drying over Na2SO4 and evaporation under reduced pressure, yielded 8.7 g of a clear, light-yellow liquid. 1H NMR (400 MHz, CDCl3) δ 1.24-1.53 (m, 10H), 4.17 (s, 4H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08722887B2 |
| 出典データセット | uspto-grants-2014_05 |
| ORD ID | ord-211e8b0ff83b457ca238a5a2e8938587 |
| 出典メモ | uspto-grants-2014_05 |