HRID627470

反应详情

EQUATION

反应方程式

HRID 627470 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
25 °C

PROCEDURE

实验过程

In a 250-mL round-bottom flask was placed a mixture of 4-bromoaniline (6.90 g, 40.1 mmol), triethylamine (16.8 g, 166 mmol), 4-dimethylaminopyridine (200 mg, 1.64 mmol), and 2-phenylacetyl chloride (6.50 g, 42.1 mmol) in dichloromethane (150 mL). The resulting mixture was stirred for 12 hours at 25° C. The reaction was then quenched by the addition of 50 mL of water. The organic layer was separated, and the aqueous layer was extracted with 2×50 mL of dichloromethane. The combined organic layers were dried over anhydrous sodium sulfate, filtered, and concentrated under vacuum. The residue was purified by flash column chromatography (silica gel column, 100:1 to 10:1 CH2Cl2/MeOH) to provide the title compound as a light yellow solid.

WORKUP

后处理

  1. customIn a 250-mL round-bottom flask was placed
  2. customThe reaction was then quenched by the addition of 50 mL of water
  3. customThe organic layer was separated
  4. extractionthe aqueous layer was extracted with 2×50 mL of dichloromethane
  5. dry with materialThe combined organic layers were dried over anhydrous sodium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated under vacuum
  8. customThe residue was purified by flash column chromatography (silica gel column, 100:1 to 10:1 CH2Cl2/MeOH)