反应 #79087
ord-1f66e7ad28ca4d44adaeddee7cd1f6bb
反应方程式
7-amino-4-methylthiopyrido[4,3-d]pyrimidine
3-methoxybenzylamine
→
7-amino-4-(3-methoxybenzylamino)pyrido[4,3-d]pyrimidine
收率 76.6%
反应条件
详细条件
See reaction.notes.procedure_details.
后处理
- 1温度at reflux for 3 h
- 2其他Evaporation of the solvent and chromatography on silica gel (5-10% EtOH/EtOAc)
实验过程
A mixture of 7-amino-4-methylthiopyrido[4,3-d]pyrimidine (136 mg, 0.71 mmol) (described in a previous experimental) and 3-methoxybenzylamine (1.37 g, 10.0 mmol) in isopropanol (3 mL) is stirred under N2 at reflux for 3 h. Evaporation of the solvent and chromatography on silica gel (5-10% EtOH/EtOAc) gives 7-amino-4-(3-methoxybenzylamino)pyrido[4,3-d]pyrimidine (153 mg, 77O) as a white solid. 1H NMR (DMSO) δ 9.11 (1H, s), 8.83 (1H, t, J=5.7 Hz), 8.26 (1H, s), 7.24 (1H, dt, Jd=0.8 Hz, Jt=8.1 Hz), 6.92 (2H, m), 6.81 (1H, dt, Jd=8.2 Hz, Jt=1.2 Hz), 6.46 (2H, brs), 6.37 (1H, s), 4.71 (2H, d, J=5.8 Hz), 3.73 (3H, s).