HRID1632773

反应详情

EQUATION

反应方程式

HRID 1632773 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A suspension of 1.85 g of 3-phthalimido-2,3-dihydro-1,5-benzoxazepin-4(5H)-one in 60 ml of absolute ethanol is treated with 0.31 ml of hydrazine hydrate and the reaction mixture is heated to reflux for 1.5 hr. After cooling to room temperature, the solid is removed by filtration and the filtrate is concentrated in vacuo. The residue is dissolved in chloroform and filtered and concentrated a second time to afford 3-amino-2,3-dihydro-1,5-benzoxazepin-4(5H)-one; m.p. 65°-70°; NMR (CDCl3) δ 6.50-7.60 (m, 4), 3.60-5.30 (m, 3), 3.25 [d (broad), 1].

WORKUP

后处理

  1. temperaturethe reaction mixture is heated
  2. temperatureto reflux for 1.5 hr
  3. customthe solid is removed by filtration
  4. concentrationthe filtrate is concentrated in vacuo
  5. dissolutionThe residue is dissolved in chloroform
  6. filtrationfiltered
  7. concentrationconcentrated a second time