HRID634071

反应详情

EQUATION

反应方程式

HRID 634071 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 43.0 g (185 mmol) of 2-(2,6-dimethylphenyl)-4,4,5,5-tetramethyl-1,3,2-dioxaborolane, 42.9 g (241 mmol) of N-bromosuccinimide, and 0.40 g (3.27 mmol) of AIBN in 1000 ml of acetonitrile was refluxed for 2 h. Then, this mixture was cooled to room temperature and evaporated to dryness. The residue was dissolved in 500 ml of hexane. The precipitate was filtered on glass frit (G3), and the filtrate was evaporated to dryness to give yellowish crystalline solid. Yield 37.9 g (66%). Anal. calc. for C14H20BBrO2: C, 54.06; H, 6.48. Found: C, 54.35; H, 6.72. 1H NMR (CDCl3): δ 7.21 (m, 1H, 4-H), 7.15 (m, 1H, 3-H), 7.07 (m, 1H, 5-H), 4.72 (s, 2H, CH2Br), 2.44 (s, 3H, 6-Me), 1.42 (s, 12H, Bpin).

WORKUP

后处理

  1. temperaturewas refluxed for 2 h
  2. customevaporated to dryness
  3. dissolutionThe residue was dissolved in 500 ml of hexane
  4. filtrationThe precipitate was filtered on glass frit (G3)
  5. customthe filtrate was evaporated to dryness
  6. customto give yellowish crystalline solid