HRID240552

反应详情

EQUATION

反应方程式

HRID 240552 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
65 °C

PROCEDURE

实验过程

To a solution of tert-butyl 4-hydroxypyridin-2-ylcarbamate (4.12 g, 19.6 mmol) and 1-fluoro-2-methyl-4-nitrobenzene (3.34 g, 21.6 mmol) in DMF (40 mL) was added K2CO3 (4.06 g, 29.04 mmol). After heating to 65° C. for 64 hours, the mixture was cooled to room temperature and poured into ice water (200 mL). The reaction mixture was extracted several times with ethyl acetate. The combined organics were concentrated under reduced pressure. The residue was chromatographed (20% ethyl acetate in hexanes) to provide the product (2.03 g, 30%).

WORKUP

后处理

  1. temperaturethe mixture was cooled to room temperature
  2. extractionThe reaction mixture was extracted several times with ethyl acetate
  3. concentrationThe combined organics were concentrated under reduced pressure
  4. customThe residue was chromatographed (20% ethyl acetate in hexanes)