HRID2202589

反应详情

EQUATION

反应方程式

HRID 2202589 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

Under a nitrogen atmosphere, 4-(tert-butyldimethylsilyloxymethyl)pyridine-1-oxide (1.2 g, 5 mmol) synthesized in Production Example 85 was dissolved in triethylamine, and trimethylsilylcyanide (744 μL, 6 mmol) was added thereto. The mixture was stirred at 90° C. for 3 hours. After the completion of the reaction was confirmed by HPLC, the reaction mixture was allowed to cool down to a room temperature. The solvent was distilled off. The resulting residue was dissolved in ethyl acetate and washed with water 3 times and with a saturated saline solution once. Thereafter, the organic layer was dried over magnesium sulfate. The solvent was distilled off, and thus the title compound (260 mg, 20.9%) was obtained as an oily substance.

WORKUP

后处理

  1. temperatureto cool down to a room temperature
  2. distillationThe solvent was distilled off
  3. dissolutionThe resulting residue was dissolved in ethyl acetate
  4. washwashed with water 3 times and with a saturated saline solution once
  5. dry with materialThereafter, the organic layer was dried over magnesium sulfate
  6. distillationThe solvent was distilled off