HRID643516

反应详情

EQUATION

反应方程式

HRID 643516 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
85 °C

PROCEDURE

实验过程

To a resealable tube was added a mixture of 3-(2-aminoquinazolin-6-yl)-4-methylpyridin-2(1H)-one (0.050 g, 0.20 mmol), potassium phosphate (0.084 g, 0.40 mmol), and copper(I) iodide (0.0075 g, 0.040 mmol) followed by Dioxane (2 mL), 1-chloro-3-iodobenzene (0.027 ml, 0.22 mmol) and N1,N2-dimethylethane-1,2-diamine (0.009 ml, 0.079 mmol). The resealable tube was purged with argon, sealed, and heated at 85° C. for 48 hrs. The crude mixture was filtered and concentrated in vacuo. The residue was purified by silica gel chromatography using 3-10% MeOH in CH2Cl2 with 1% NH4OH to afford 3-(2-amino-6-quinazolinyl)-1-(3-chlorophenyl)-4-methyl-2(1H)-pyridinone as an off-white solid. M+H+=363.1.

WORKUP

后处理

  1. additionTo a resealable tube was added
  2. customThe resealable tube was purged with argon
  3. customsealed
  4. filtrationThe crude mixture was filtered
  5. concentrationconcentrated in vacuo
  6. customThe residue was purified by silica gel chromatography