HRID427666

反应详情

EQUATION

反应方程式

HRID 427666 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

A solution of 5-(tert-butyldimethylsilyloxy)-2-phthalimidoaniline (1.02 g, 2.77 mmol) in toluene (15 mL) was treated with a solution of 20% phosgene in toluene (2 mL) at reflux for 20 min. The volatile materials were removed in vacuo to give a tan solid, which was dissolved in dry methylene chloride (20 mL) and treated with 1-(4-pyridyl)piperidine-4-methanol (0.53 g, 2.77 mmol). The resulting suspension was stirred for 90 min then diluted with hexane. The mixture was allowed to stand overnight and the resulting precipitate collected by vacuum filtration and dried to yield 1.46g (90%) of the title compound as a tan powder.

WORKUP

后处理

  1. temperatureat reflux for 20 min
  2. customThe volatile materials were removed in vacuo
  3. customto give a tan solid, which
  4. waitto stand overnight
  5. filtrationthe resulting precipitate collected by vacuum filtration
  6. customdried