HRID510829

反应详情

EQUATION

反应方程式

HRID 510829 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 1-(3-bromo-5-chloro-2-methoxy-4-methylphenyl)ethanone (3.3 g, 12 mmol), N-bromosuccinimide (2.2 g, 13 mmol), and benzoyl peroxide (0.15 g, 0.60 mmol) in carbon tetrachloride (50 mL) was heated at reflux overnight. The mixture was cooled to room temperature and concentrated. The resulting residue was diluted with ethyl acetate and washed with water. The organic layers were dried over magnesium sulfate and evaporated to dryness. The crude product was used directly in next step. LCMS calculated for C10H10Br2ClO2 (M+H)+: m/z=355.1. found: 355.1.

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureat reflux overnight
  3. concentrationconcentrated
  4. additionThe resulting residue was diluted with ethyl acetate
  5. washwashed with water
  6. dry with materialThe organic layers were dried over magnesium sulfate
  7. customevaporated to dryness