反应详情

Leave the following under hydrogen pressure (Patm) for 48 hours: 80 mg of 5-(1,1′-biphenyl-4-yl)-1-ethyl-7,8-dimethoxy-1,3-dihydro-2H-1,4-benzodiazepin-2-one (IIbp), 16 mg of 10% palladium on charcoal (20% by weight of product to reduce), in 30 ml of methanol and 1 ml of CH2Cl2. Filter on celite, rinse several times with methanol. Evaporate to dryness. Purify by silica chromatography (AcOEt 1/hexane 1). Recrystallize in ether. One obtains 28 mg of the abovenamed product in the form of a white powder. Yield: 35%. M: 148–150° C. 1H-NMR (CDCl3, 200 MHz): d 1.27 (t, 3H, —CH3), 3.00 (s, 4H, 2×—CH2). 3,37–3,40 (m, 2H, CH2), 3.45–3.65 (m, 4H, —OCH3+1H NCH2), 3.92 (s, 3H, OCH3), 4.21–4.48 (m, 1H, NCH2), 6.22 (d, 1H Ar), 6.77 (d, 1H Ar), 7.19–7.39 (m, 9H Ar).

1. filtrationFilter on celite
2. washrinse several times with methanol
3. customEvaporate to dryness
4. customPurify by silica chromatography (AcOEt 1/hexane 1)
5. customRecrystallize in ether