HRID446276

反应详情

EQUATION

反应方程式

HRID 446276 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
95 °C

PROCEDURE

实验过程

4-(2-Chloro-pyridin-3-yl)-pyrimidine (10.4 g, 54 mmol), 3-amino-4-methylbenzoic acid (19.4 g, 128 mmol), 17 g Et3N-TFA salt (The liquid Et3N-TFA reagent was generated by adding 2.5 mL TFA dropwise to a 0° C. solution of 3 mL Et3N in isopropanol, then concentrating by rotary evaporator followed by 30 minutes under high vacuum.), and 15 mL DMSO were mixed together in a sealed tube under argon. The mixture was stirred at 95° C. for 65 h. After cooling to RT, the residue was sonicated in 100 mL methanol to break up the solids, then filtered to obtain product as a yellow solid. MS m/z=307 [M+H]+. Calc'd for C17H14N4O2: 306.33.

WORKUP

后处理

  1. concentrationconcentrating by rotary evaporator
  2. addition), and 15 mL DMSO were mixed together in a sealed tube under argon
  3. temperatureAfter cooling to RT
  4. customthe residue was sonicated in 100 mL methanol
  5. filtrationfiltered
  6. customto obtain product as a yellow solid