HRID36318

反应详情

EQUATION

反应方程式

HRID 36318 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. customIn a round bottom flask equipped with a magnetic stirrer, nitrogen inlet
  2. temperaturereflux condenser
  3. customdrying tube
  4. temperatureThe reaction mixture was heated by an oil bath at 95°-100° C. for 4 hours
  5. filtrationfiltered
  6. distillationThe filtrate was distilled with a short path distillation apparatus
  7. customthe product was collected at 160°-163° C. at 29 mm Hg
  8. customto give a pale yellow solid, m.p. 104°-106° C