HRID1499117

反应详情

EQUATION

反应方程式

HRID 1499117 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

To a solution of (R)-1-(2-bromo-4-chlorophenyl)-2,2,2-trifluoroethanol (300 mg, 1.1 mmol) in dioxane (12 mL) was added phenyl boronic acid (185 mg, 1.5 mmol), Pd2(dppf)Cl2 (35 mg, 0.07 mmol) and Na2CO3 (3 mL, 2.0 M, aq). The reaction was heated to 90° C. for 2 h, then cooled to RT, and concentrated in vacuo. The residue was taken up in CH2Cl2, washed with brine, and extracted with CH2Cl2. The combined organic layers were dried over Na2SO4. Purification by normal phase silica gel column (EtOAc/hexanes) to provide a white solid.

WORKUP

后处理

  1. temperaturecooled to RT
  2. concentrationconcentrated in vacuo
  3. washwashed with brine
  4. extractionextracted with CH2Cl2
  5. dry with materialThe combined organic layers were dried over Na2SO4
  6. customPurification by normal phase silica gel column (EtOAc/hexanes)
  7. customto provide a white solid