2,3-Dihydrobenzo[b]oxepine → HCID 13149080, 화합물

HRID 1431958노트

반응식

HRID 1431958 반응식
[O:1]1[C:7]2[CH:8]=[CH:9][CH:10]=[CH:11][C:6]=2[CH:5]=[CH:4][CH2:3][CH2:2]1.C(=O)([O-])[OH:13].[Na+].OOS([O-])=O.[K+]>C(OCC)(=O)C.O.O>[O:13]1[CH:5]2[CH:4]1[CH2:3][CH2:2][O:1][C:7]1[CH:8]=[CH:9][CH:10]=[CH:11][C:6]=12

참가 물질

6

반응물 3

HCID 2567432,3-Dihydrobenzo[b]oxepineHCID 516892Sodium BicarbonateHCID 23707502Potassium hydroxy sulfite

생성물 1

HCID 13149080HCID 13149080, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 22728543Water ethylacetate용매

실험 절차

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.

후처리

  1. additionAfter the end of the addition
  2. waitis carried out for a further hour
  3. customthe organic phase is separated off
  4. extractionThe aqueous phase is again extracted with 10 ml of ethyl acetate
  5. washthe combined organic phases are washed with water
  6. customdried
  7. filtrationfiltered
  8. customevaporated to dryness

출처 및 근거

ORD 기록
ord-3e532449bb03439a94a3b1bbb236a6bb
출처 데이터셋
uspto-grants-2009_11
특허 번호
US07612061B2

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