2,3-Dihydrobenzo[b]oxepine → HCID 13149080、化合物

HRID 1431958ノート

反応式

HRID 1431958 の反応式
[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

参加物

6

反応物 3

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

生成物 1

HCID 13149080HCID 13149080、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 22728543Water ethylacetate溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-3e532449bb03439a94a3b1bbb236a6bb
出典データセット
uspto-grants-2009_11
特許番号
US07612061B2

反応ノート

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