HRID522902

反应详情

EQUATION

反应方程式

HRID 522902 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

To 2,4-dichloropyrimidine (250.0 mg, 1.678 mmol) and 3-amino-N-methylbenzamide (252 mg, 1.678 mmol) in 2-propanol (8390 μL) in a disposable sealed tube at RT was added N-ethyl-N-isopropylpropan-2-amine (585 μL, 3.36 mmol). The resulting reaction mixture was heated at 60° C. for 22 h, then to 70° C. for 23 h, then 80° C. for 3 days, cooled to RT, concentrated, purified using MPLC (5 g cartridge, 12 g column, 0 to 60% 90/10 CH2Cl2-MeOH in CH2Cl2) giving 3-(2-chloropyrimidin-4-ylamino)-N-methylbenzamide (389.0 mg).

WORKUP

后处理

  1. customThe resulting reaction mixture
  2. wait80° C. for 3 days
  3. temperaturecooled to RT
  4. concentrationconcentrated
  5. custompurified