反应详情

温度

50 °C

Azide 23 (Example 10, 50 mg, 0.11 mmol) is dissolved in 1 mL methanol, and 2 mL methylamine (33% in ethanol) are added. The reaction mixture is stirred at 50° C. over night and all volatiles are removed in vacuo. The product is purified by flash column chromatography (CH2Cl2/MeOH 10:1) to yield 33.5 mg. 1H-NMR (400 MHz, DMSO-d6): δ=7.85 (s, 1H, H-8), 7.41, (d, J=8.1, 2H, ArH), 7.35 (d, J=8.1, 2H, ArH), 6.44 (s br, 2H, NH2), 5.44 (s, 2H, OCH2), 4.05 (t, J=, 2H, CH2), 3.72 (s, 2H, CH2), 3.35 (t, J=6.5, 2H, CH2), 1.99 (m, 2H, CH2) ppm. MS (ESI) m/z 354.1 [M+H]+.

1. customall volatiles are removed in vacuo
2. customThe product is purified by flash column chromatography (CH2Cl2/MeOH 10:1)
3. customto yield 33.5 mg