反应详情

温度

50 °C

Stir for 12 hours under an inert atmosphere at 50° C., a mixture of 100 mg (0.27 mmol) of 5-(4-bromophenyl)-1-ethyl-7,8-dimethoxy-1,3-dihydro-2H-1,4-benzodiazepin-2-one (IIbl), 194 mg (1.3 mmol) of [(prop-2-ynyloxy)methyl]benzene, 9.0 mg of CuI, 5.2 mg of PdCl2, 18.0 mg of PPh3, 0.5 ml of TEA, 2 ml of CH3CN. Evaporate to dryness and purify by silica chromatography (AcOEt 1/hexane 1). Recrystallize in EtO2/pentane. Yield: 37%. M: 64–66° C. 1H-NMR (CDCl3, 300 MHz): d 1.12 (s, 3H, CH3), 3.72–3.83 (m, 4H, 1H CH2+OCH3), 4.00 (AB system, ? d=0.63, JAB=13.5, 2H, —NCH2), 4.03 (s, 3H, OCH3), 4.43 (s, 2H, OCH2), 4.69 (m, 2H, ═C—CH2), 4.77 (m, 1H, OCH2), 6.65 (s, 1H Ar), 6.86 (s, 1H Ar), 7.27–7.63 (m, 9H Ar).

1. customEvaporate to dryness
2. custompurify by silica chromatography (AcOEt 1/hexane 1)
3. customRecrystallize in EtO2/pentane
4. custom64–66° C