HRID921505

反应详情

EQUATION

反应方程式

HRID 921505 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To the solution of 6-hydroxy-4,4,5,7,8-pentamethylchroman-2-one (15 g, 0.064 mol) in a mixture of acetonitrile (600 ml), acetone (50 ml) and water (300 ml), NBS (11.4 g, 0.064 mol) was added. The resultant mixture was stirred for 30 minutes at room temperature. After removing most of the organic solvent, the yellow solid was collected by filtration, washed by water and dried over vacuum to afford a yield of 96%. 1H NMR (300 MHz, CD2Cl2) δ 3.0 (s, 2H, CH2), 2.13 (s, 3H, CH3), 1.94 (s, 3H, CH3), 1.92 (s, 3H, CH3), 1.44 (s, 6H, CH3); MS (m/e): 251 (M+).

WORKUP

后处理

  1. additionwas added
  2. customAfter removing most of the organic solvent
  3. filtrationthe yellow solid was collected by filtration
  4. washwashed by water
  5. customdried over vacuum
  6. customto afford a yield of 96%