反应 #79087

ord-1f66e7ad28ca4d44adaeddee7cd1f6bb

反应方程式

CSc1ncnc2cc(N)ncc12
7-amino-4-methylthiopyrido[4,3-d]pyrimidine
COc1cccc(CN)c1
3-methoxybenzylamine
COc1cccc(CNc2ncnc3cc(N)ncc23)c1
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. 1
    温度at reflux for 3 h
  2. 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).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US06713484B2uspto-grants-2004_03