HRID2422733

反应详情

EQUATION

反应方程式

HRID 2422733 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

A mixture of (1R)-1-[2-(3-methylphenyl)-2H-tetrazol-5-yl]ethanol (251 mg, 1.23 mmol), 2-[4-methyl-5-(methylsulfonyl)-4H-1,2,4-triazol-3-yl]pyrimidine (239 mg, 1.00 mmol) and cesium carbonate (911 mg, 2.80 mmol) in N,N-dimethylformamide (10 mL) was stirred at 65° C. for 15 h. After cooling to room temperature, the product was partitioned between ethyl acetate (300 mL) and water (50 mL). The organic layer was washed with water (3×50 mL) and brine (50 mL), and dried over sodium sulfate. The solvent was concentrated in vacuo. Flash chromatography (silica gel, 2-3% methanol in dichloromethane) yielded the title compound (265 mg, 73%, oil).

WORKUP

后处理

  1. temperatureAfter cooling to room temperature
  2. customthe product was partitioned between ethyl acetate (300 mL) and water (50 mL)
  3. washThe organic layer was washed with water (3×50 mL) and brine (50 mL)
  4. dry with materialdried over sodium sulfate
  5. concentrationThe solvent was concentrated in vacuo