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
PROCEDURE
实验过程
In a round bottom flask equipped with a magnetic stirrer, nitrogen inlet, reflux condenser and drying tube were placed 5-methoxycarbonylbenzoxazolthione (5.2 g, 0.025 mole), phosphorus pentachloride (5.2 g, 0,025 mole), and phosphorus oxychloride (40 mL). The reaction mixture was heated by an oil bath at 95°-100° C. for 4 hours. The reaction mixture was allowed to cool to room temperature and filtered. The filtrate was distilled with a short path distillation apparatus and the product was collected at 160°-163° C. at 29 mm Hg. The product solidified on standing to give a pale yellow solid, m.p. 104°-106° C. Anal Calcd. for C9H6ClNO3: C, 51.1; H, 2.9; N, 6.6; Cl, 16.8. Found: C, 50.7; H, 2.9; N, 6.6; Cl, 16.3
WORKUP
后处理
- customIn a round bottom flask equipped with a magnetic stirrer, nitrogen inlet
- temperaturereflux condenser
- customdrying tube
- temperatureThe reaction mixture was heated by an oil bath at 95°-100° C. for 4 hours
- filtrationfiltered
- distillationThe filtrate was distilled with a short path distillation apparatus
- customthe product was collected at 160°-163° C. at 29 mm Hg
- customto give a pale yellow solid, m.p. 104°-106° C