HRID1070392

反应详情

EQUATION

反应方程式

HRID 1070392 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
85 °C

PROCEDURE

实验过程

To a solution of methyl 2-amino-5-bromobenzoate (2.0 g, 8.7 mmol) in dioxane (40 mL) were added phenylboronic acid (1.91 g, 15.7 mmol), potassium phosphate (4.08 g, 19.1 mmol) and tetrakis(triphenylphosphine)palladium (0.26 g, 0.22 mmol) under nitrogen. The mixture was heated at 85° C. for 20 h, then cooled to 0-5° C. Aqueous ammonium chloride was added and the mixture was extracted, washed with brine, dried (Na2SO4) and concentrated to dryness. Purification by chromatography gave 1.45 g of methyl 2-amino-5-phenylbenzoate.

WORKUP

后处理

  1. temperaturecooled to 0-5° C
  2. extractionthe mixture was extracted
  3. washwashed with brine
  4. dry with materialdried (Na2SO4)
  5. concentrationconcentrated to dryness
  6. customPurification by chromatography