HRID220813

反应详情

EQUATION

反应方程式

HRID 220813 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperatureThe mixture was heated
  2. temperatureat reflux for 20 h
  3. concentrationthen concentrated in vacuo
  4. customazeotroped with toluene
  5. dissolutionThe residue was dissolved in diethyl ether
  6. customthe layers were partitioned
  7. washThe organic layer was washed with brine
  8. customdried
  9. concentrationconcentrated in vacuo