HRID2287727

反应详情

EQUATION

反应方程式

HRID 2287727 的结构方程式

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

A mixture of 4-methylthiopyrido[3,4-d]pyrimidine (75 mg, 0.42 mmol), and aniline (1 mL) is heated to 100° C. under N2 for 2 h. The reaction mixture is then chromatographed on silica using MPLC and eluting with a gradient system (CHCl3 to 5% MeOH in CHCl3). The fractions are concentrated under reduced pressure, and the resulting solid is recrystallized from Et2O to yield 4-anilinopyrido[3,4-d]pyrimidine (21.2 mg, 23%) as a yellow solid. 1H NMR (DMSO) δ 10.09 (1H, s), 9.18 (1H, s), 8.74 (1H, d, J=5.3 Hz), 8.46 (1H, d, J=5.8 Hz), 7.89 (2H, d, J=8.5 Hz), 7.45 (2H, t, J=7.9 Hz), 7.21 (1H, t, J=7.4 Hz).

WORKUP

后处理

  1. customThe reaction mixture is then chromatographed on silica using MPLC
  2. washeluting with a gradient system (CHCl3 to 5% MeOH in CHCl3)
  3. concentrationThe fractions are concentrated under reduced pressure
  4. customthe resulting solid is recrystallized from Et2O