HRID1596156

反应详情

EQUATION

反应方程式

HRID 1596156 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of N,N-ditetradecyl-p-toluenesulfonamide (4.16 g; 7.38 mmol) in tetrahydrofuran (2 ml) is added at 0° C. to a solution of lithium naphthalenide [prepared from naphthalene (4.73 g; 36.88 mmol) and lithium metal (0.38 g; 55.35 mmol) in tetrahydrofuran (40 ml) at room temperature for 1 h] and the reaction mixture is stirred for 1 h at room temperature. Methanol (2 ml) is added, followed by water (25 ml) and the mixture is extracted with ether (2×25 ml). The organic phase is dried over sodium sulfate, filtered and concentrated under reduced pressure to give a white solid which is purified by chromatography on a column of silica gel (eluent: ether) to give ditetradecylamine (2.68 g; 89%).

WORKUP

后处理

  1. extractionthe mixture is extracted with ether (2×25 ml)
  2. dry with materialThe organic phase is dried over sodium sulfate
  3. filtrationfiltered
  4. concentrationconcentrated under reduced pressure
  5. customto give a white solid which
  6. customis purified by chromatography on a column of silica gel (eluent: ether)