HRID1011287

反应详情

EQUATION

反应方程式

HRID 1011287 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
130 °C

PROCEDURE

实验过程

To a sealed tube equipped with a magnetic stir bar was added 4-chloro-7H-pyrrolo[2,3-d]pyrimidine (1.0 g, 6.5 mmol, 1.0 eq.), 2-Fluoro-4-nitro-phenol (1.5 g, 9.5 mmol, 1.5 eq) and bromobenzene (5 ml). The mixture was stirred at 130° C. for 4 hours. The reaction mixture was then cooled to room temperature and ether was added (5 ml). After addition of ether the resulting precipitate was filtered and washed with ether. The product was recrystallized from methanol to give 4-(2-fluoro-4-nitro-phenoxy)-7H-pyrrolo[2,3-d]pyrimidine as an off white solid. (1.6 g, 89% yield). 1H NMR (400 MHz, DMSO): 12.44 (s, 1H), 8.41(dd, 1H), 8.34 (s, 1H), 8.24 (m, 1H), 7.80 (m, 1H), 7.61 (m, 1H), 6.69 (d, 1H); MS (ESI) for C12H7FN4O3: 275 (MH+).

WORKUP

后处理

  1. customTo a sealed tube equipped with a magnetic stir bar
  2. temperatureThe reaction mixture was then cooled to room temperature
  3. filtrationwas filtered
  4. washwashed with ether
  5. customThe product was recrystallized from methanol