反应 #669944

ord-9029bb612df649a88c69c323defe5ca9

反应条件

温度
5°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度is maintained at 5° C
  2. 2
    workup.WAITThe mixture is left
  3. 3
    workup.STIRRINGstirring for one and a half hours at RT
  4. 4
    过滤filtered
  5. 5
    其他the residue is dried under vacuum

实验过程

1 g of NaNO2 is added to a solution of 3 g of the acid obtained in step A in 10 ml of water and 2 ml of 30% sodium hydroxide. This solution is poured over 1 hour into 10 ml of concentrated HCl cooled to 5° C. After stirring for 3 hours at 5° C., a solution of 7.5 g of SnCl2.2H2O in 15 ml of concentrated HCl is added slowly while the temperature is maintained at 5° C. The mixture is left stirring for one and a half hours at RT and filtered, and the residue is dried under vacuum to obtain 2.86 g of the expected product.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US05925661uspto-grants-1999_07