HRID386390
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
- 79 °C
PROCEDURE
实验过程
To a solution of 1-naphthalenylisothiocyanate (500 mg, 2.7 mmol) in ethanol (150 mL) was added sodium azide (2.8 g, 43 mmol) and the mixture was heated to 79° C. for 2 hours. The reaction mixture was then cooled to room temperature, aqueous HCl solution (12N, 1.5 mL) added and the mixture concentrated. The resulting residue was diluted with ethyl acetate and extracted with aqueous NaOH solution (1N) and the aqueous layer acidified with aqueous HCl solution (12N) until a precipitate formed. The precipitate was collected and used in the next step without further purification (520 mg, 85% yield).
WORKUP
后处理
- temperatureThe reaction mixture was then cooled to room temperature
- concentrationthe mixture concentrated
- additionThe resulting residue was diluted with ethyl acetate
- extractionextracted with aqueous NaOH solution (1N)
- customformed
- customThe precipitate was collected
- customused in the next step without further purification (520 mg, 85% yield)