Hydrogen Peroxide → 2,3-Diaza-spiro[4.5]dec-2-ene
반응식
[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]1참가 물질
6
실험 절차
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).
후처리
- 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
출처 및 근거
- ORD 기록
- ord-211e8b0ff83b457ca238a5a2e8938587
- 출처 데이터셋
- uspto-grants-2014_05
- 특허 번호
- US08722887B2
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