反应详情

Stir a mixture of 80 mg (0.24 mmol) of 7,8-dimethoxy-1-methyl-5-(2-phenylethynyl)-1,3-dihydro-1,4-benzodiazepin-2-one 132, 15 mg of 10% Pd/C by weight in 5 ml of MeOH and 5 ml of CH2Cl2 under 70 psi of H2 for 48 hours. Filter the suspension on celite, rinse three times with 10 ml of MeOH. Evaporate to dryness and purify by silica chromatography (AcOEt 1/hexane 1, then AcOEt). Yield: 5%. M: 112–115° C. 1H-NMR (CDCl3, 300 MHz): d 2.95–3.07 (m, 4H, CH2CH2), 3.28 (s, 3H, NCH3), 3.87 (s, 3H, OCH3), 3.93 (s, 3H, OCH3), 4.10 (AB system, ? d=0.96, JAB=10.2, 2H, CH2), 6.67 (s, 1H Ar), 6.78 (s, 1H Ar), 7.15–7.25 (m, 5H Ar). Mass: (M+H)+=339.15

1. filtrationFilter the suspension on celite
2. washrinse three times with 10 ml of MeOH
3. customEvaporate to dryness
4. custompurify by silica chromatography (AcOEt 1/hexane 1
5. custom112–115° C