HRID838879

反应详情

EQUATION

反应方程式

HRID 838879 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 62 g (0.61 mole) of 3-amino-2-oxazolidone in 650 ml of benzene was treated with 15 drops of HCl (isopropanol) solution using mechanical stirring, and refluxed until all water was removed via a Dean-Stark trap. The solution was then treated with 107 g (0.60 mole) of 6-methoxy-4-chromanone and refluxed for 11.5 hr. A 9.6 ml portion of water (theory: 10.8 ml) was collected. The reaction mixture was stripped of benzene under the water pump. The residue was taken up in 200 ml of 1:1 isopropanol:ether, stored 24 hr at room temperature, refrigerated overnight and filtered. The resultant cream-colored solid was washed with 125 ml of isopropanol, ether, and dried. M.p. 54°-64°; yield: 115 g (73%).

WORKUP

后处理

  1. customwas removed via a Dean-Stark trap
  2. temperaturerefluxed for 11.5 hr
  3. customA 9.6 ml portion of water (theory: 10.8 ml) was collected
  4. filtrationfiltered
  5. washThe resultant cream-colored solid was washed with 125 ml of isopropanol, ether
  6. customdried