HRID17760

反应详情

EQUATION

反应方程式

HRID 17760 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of trityl chloride (4.6 g, 17 mmol) and diisopropylethylamine (DIEA, 4.2 g, 33 mmol) in toluene (50 mL) was added 11-mercaptoundecanoic acid, 1 (6.0 g, 14 mmol), and the solution was stirred at room temperature for 3 h. The solution was evaporated, and the product separated between dichloromethane and water. The organic phase was washed with water (2×100 mL), dried (MgSO4), filtered, and concentrated to yield crude 2 (6.3 g, 13.6 mmol, 97%). 1H NMR (CDCl3, 500 MHz): δ1.14-1.42 (br m, 14H), 1.59-1.68 (br t, 2H), 2.06-2.09 (br m, 2H), 2.36-2.40 (t, 2H), 7.19-7.23 (m, 6H), 7.26-7.29 (m, 9H).

WORKUP

后处理

  1. customThe solution was evaporated
  2. customthe product separated between dichloromethane and water
  3. washThe organic phase was washed with water (2×100 mL)
  4. dry with materialdried (MgSO4)
  5. filtrationfiltered
  6. concentrationconcentrated