HRID1632773
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
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
- temperaturethe reaction mixture is heated
- temperatureto reflux for 1.5 hr
- customthe solid is removed by filtration
- concentrationthe filtrate is concentrated in vacuo
- dissolutionThe residue is dissolved in chloroform
- filtrationfiltered
- concentrationconcentrated a second time