HRID1482663

反应详情

EQUATION

反应方程式

HRID 1482663 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
120 °C

PROCEDURE

实验过程

In a 50 mL 3-neck RBF equipped with N2 bubbler and reflux condenser 2,4-dichloro-5-fluoropyrimidine (1.79 g) in 1-butanol (20 mL), 4-nitroaniline (1.0 g) and DIPEA (2.6 mL) were charge at room temperature. The reaction mixture was heated to 120° C. for 2 hr. The reaction was monitored on TLC using hexane:ethyl acetate (8:2) as mobile phase. After completion, the reaction mixture was cooled to room temperature. Solid precipitate was filtrated and washed with cold hexanes and dried to give 1.26 g of 2-chloro-5-fluoro-N-(3-nitrophenyl)pyrimidin-4-amine.

WORKUP

后处理

  1. additionwere charge at room temperature
  2. temperatureAfter completion, the reaction mixture was cooled to room temperature
  3. filtrationSolid precipitate was filtrated
  4. washwashed with cold hexanes
  5. customdried