反应 #1519140

ord-3e532449bb03439a94a3b1bbb236a6bb

反应方程式

O=S([O-])OO.[K+]
Oxone
O=C([O-])O.[Na+]
sodium hydrogen carbonate
C1=Cc2ccccc2OCC1
2,3-dihydro-1-benzoxepin
c1ccc2c(c1)OCCC1OC21
expected product
c1ccc2c(c1)OCCC1OC21
1a,2,3,8b-Tetrahydrooxireno[d][1]benzoxepin

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    workup.ADDITIONAfter the end of the addition
  2. 2
    workup.WAITis carried out for a further hour
  3. 3
    其他the organic phase is separated off
  4. 4
    萃取The aqueous phase is again extracted with 10 ml of ethyl acetate
  5. 5
    洗涤the combined organic phases are washed with water
  6. 6
    其他dried
  7. 7
    过滤filtered
  8. 8
    其他evaporated to dryness

实验过程

To 0.5 g of 2,3-dihydro-1-benzoxepin (3.42 mmol), prepared according to the method described in J. Org. Chem., 1969, 34 (1), 207, dissolved in 30 ml of a mixture of ethyl acetate/water 50/50, there are added 1.44 g of sodium hydrogen carbonate (17.1 mmol) and then, over 1 hour, a solution of 2.1 g of Oxone® (3.42 mmol) in 15 ml of water. After the end of the addition, stirring is carried out for a further hour and then the organic phase is separated off. The aqueous phase is again extracted with 10 ml of ethyl acetate, and the combined organic phases are washed with water, dried, filtered and evaporated to dryness to yield the expected product in the form of an oil.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07612061B2uspto-grants-2009_11