反应详情

Tri-tert-butyl 2,2′,2″-(1,4,7,10-tetraazacyclododecane-1,4,7-triyl)triacetate (33.5 mg, 65.1 mop was dissolved in dry CH3CN (10 mL) and magnetically stirred under N2(g). Anhydrous K2CO3 (30.0 mg, 0.217 mmol) was added, followed by 2-chloro-N-(phenanthridin-6-ylmethyl)acetamide (Weitz et al., J. Am. Chem. Soc., 2012, 134, 16099-16102) (15.4 mg, 54.2 mmol) dissolved in 15 mL CH3CN/DMF (2:1), and the reaction mixture was heated to reflux for 27 hours under N2(g). The reaction mixture was then filtered and concentrated under reduced pressure to yield a colorless glass that was used without further purification in the next step. 1H NMR (500 MHz, CDCl3) δ 1.45 (s, 27H), 2.70-3.21 (m, 16H), 3.37-3.42 (m, 6H), 5.41 (d, J=15 Hz, 2H), 7.66-7.87 (m, 3H), 8.02 (d, J=7.0 Hz, 1H), 8.22 8.28 (d, J=6.5 Hz, 1H), 8.55 (d, J=8.0 Hz, 1H), 8.63 (d, J=7.5 Hz, 1H), 8.77 (d, J=7.0 Hz, 1H). HRMS (ESI): calc for [C42H62N6O7]+ ([M+H]+): m/z 763.4753. found: 763.4739.

1. temperaturethe reaction mixture was heated
2. temperatureto reflux for 27 hours under N2(g)
3. filtrationThe reaction mixture was then filtered
4. concentrationconcentrated under reduced pressure
5. customto yield a colorless glass that
6. customwas used without further purification in the next step