反应详情

温度

110 °C

Heat at 110° C. in a sealed tube a mixture of 100 mg (0.37 mmol) of 5-chloro-7,8-dimethoxy-1-methyl-1,3-dihydro-1,4-benzodiazepin-2-one XVIIIaa and 300 μl (3 mmol) of piperidine in 10 ml of EtOH for 48 hours. Evaporate to dryness and purify by silica chromatography (CH2Cl2 50/AcOEt 40/EtOH 10). Triturate in hexane, filter, dry. One obtains 70 mg of a beige powder. Yield: 60%. M=125–127° C. 1H-NMR (200 MHz, DMSO): δ 1.63–1.70 (m, 6H, 3×CH2), 3.20–3.23 (m, 4H, 2×CH2), 3.37 (s, 3H, NCH3), 3.91 (AB system, Δδ=0.71, JAB=11.5, 2H, 3-CH2), 3.94 (s, 3H, OCH3), 3.97 (s, 3H, OCH3), 6.73 (s, 1H Ar), 6.99 (s, 1H Ar).

1. customEvaporate to dryness
2. custompurify by silica chromatography (CH2Cl2 50/AcOEt 40/EtOH 10)
3. customTriturate in hexane
4. filtrationfilter
5. customdry