HRID220813
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
(3-Chloro-7,8-dihydro-6H-5-oxa-9-aza-benzocyclohepten-9-yl)-phenyl-methanone from Example E25.2 (783 mg, 2.7 mmol) was dissolved in dioxan (10 ml) and 6M HCl aqueous solution (50 ml) was added. The mixture was heated at reflux for 20 h then concentrated in vacuo and azeotroped with toluene. The residue was dissolved in diethyl ether and water, basified with NaHCO3 and the layers were partitioned. The organic layer was washed with brine, dried and concentrated in vacuo to yield the title compound (280 mg, 47%).
WORKUP
后处理
- temperatureThe mixture was heated
- temperatureat reflux for 20 h
- concentrationthen concentrated in vacuo
- customazeotroped with toluene
- dissolutionThe residue was dissolved in diethyl ether
- customthe layers were partitioned
- washThe organic layer was washed with brine
- customdried
- concentrationconcentrated in vacuo