反应 #44486

ord-e58910d5be334e0b8fdc14a5c87f8aa6

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他The solvent was evaporated in vacuo
  2. 2
    workup.STIRRINGstirred at room temperature for two hours
  3. 3
    其他The reaction was quenched with 10% sodium bisulfite
  4. 4
    萃取extracted with dichloromethane
  5. 5
    洗涤The organic phase was washed with water
  6. 6
    干燥dried with MgSO4
  7. 7
    过滤filtered
  8. 8
    其他evaporated in vacuo

实验过程

To a solution of Example 1D (0.168 mg, 0.475 mmoles) in methanol (1.5 mL), two drops of 12M HCl was added and stirred for one hour. The solvent was evaporated in vacuo. The residue was taken in dichloromethane (2.5 mL) and Dess-Martin periodinane (0.25 gm, 0.593 mmoles) was added and stirred at room temperature for two hours. The reaction was quenched with 10% sodium bisulfite and extracted with dichloromethane. The organic phase was washed with water, dried with MgSO4, filtered, and evaporated in vacuo to provide the title compound.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07737137B2uspto-grants-2010_06