HRID928552

反应详情

EQUATION

反应方程式

HRID 928552 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

To a stirred solution of 6-bromo-4-fluoro-2,3-dinitrophenol (4.4 g, 16 mmol) in methanol (88 mL) and 12.0 M hydrogen chloride in water (40 mL) was added stannous chloride, dihydrate (11 g, 47 mmol). The reaction was stirred at RT for 15 min. Water was added and the mixture was extracted with ethyl acetate. The organic layer was separated and concentrated. Purification on silica gel using ethyl acetate in hexanes gave the desired compound, 2.48 g, 63%. 1H NMR (300 MHz, DMSO-d6) δ 9.80 (br s, 3H), 6.80 (m, 1H).

WORKUP

后处理

  1. extractionthe mixture was extracted with ethyl acetate
  2. customThe organic layer was separated
  3. concentrationconcentrated
  4. customPurification on silica gel