Hydrogen Peroxide → 2,3-Diaza-spiro[4.5]dec-2-ene
反応式
[NH2:1][CH2:2][C:3]1([CH2:9][NH2:10])[CH2:8][CH2:7][CH2:6][CH2:5][CH2:4]1.OO.[O-]Cl.[Na+]>O.CO>[CH2:2]1[C:3]2([CH2:8][CH2:7][CH2:6][CH2:5][CH2:4]2)[CH2:9][N:10]=[N:1]1参加物
6
実験手順
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).
後処理
- temperaturecooled in an ice bath
- customthe ice bath was removed
- extractionExtraction with DCM
- dry with materialdrying over Na2SO4 and evaporation under reduced pressure
- customyielded 8.7 g of a clear, light-yellow liquid
出典と根拠
- ORDレコード
- ord-211e8b0ff83b457ca238a5a2e8938587
- 出典データセット
- uspto-grants-2014_05
- 特許番号
- US08722887B2
反応ノート
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