HRID2354134

反应详情

EQUATION

反应方程式

HRID 2354134 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

A mixture of 7-(4-formylphenyl)-6-phenylpyrido[2,3-d]pyrimidine-2-carboxamide (2-6) (0.033 g, 0.093 mmol), 3-oxo-3-phenylpropan-1-aminium chloride (0.031 g, 0.168 mmol), and TEA (0.023 mL, 0.168 mmol) in 5% CH3COOH in DMF (0.5 mL) was stirred for 4 hr at which point NaBH(OAc)3 (0.039 g, 0.186 mmol) was added. The mixture was stirred for a 30 min. further. 2 drops of water were added and the material was purified by reverse phase HPLC. 1H-NMR (500 MHz, d6-DMSO) δ 9.90 (s, 1H), 8.88 (bs, 2H), 8.79 (s, 1H), 8.43 (s, 1H), 7.99 (d, 3H, J=7.3 Hz), 7.70 (t, 1H, J=7.1 Hz), 7.62-7.53 (m, 3H), 7.50 (d, 2H, J=8.3 Hz), 7.43-7.31 (m, 6H), 4.31-4.34 (m, 2H), 3.50 (t, 2H, J=6.6 Hz), 3.36-3.26 (m, 2H); LRMS, calc'd: 488.1; found 488.1.

WORKUP

后处理

  1. additionwas added
  2. customthe material was purified by reverse phase HPLC