反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureto cool down to a room temperature
- distillationThe solvent was distilled off
- dissolutionThe resulting residue was dissolved in ethyl acetate
- washwashed with water 3 times and with a saturated saline solution once
- dry with materialThereafter, the organic layer was dried over magnesium sulfate
- distillationThe solvent was distilled off