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Sodium Carbonate → 7-Methoxy-3,4-dihydro-1-benzoxepin-5-one oxime

HRID 1448062
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HRID 1448062 반응식
Cl.[NH2:2][OH:3].C(=O)([O-])[O-].[Na+].[Na+].[CH3:10][O:11][C:12]1[CH:13]=[CH:14][C:15]2[O:21][CH2:20][CH2:19][CH2:18][C:17](=O)[C:16]=2[CH:23]=1>O.C(O)C>[CH3:10][O:11][C:12]1[CH:13]=[CH:14][C:15]2[O:21][CH2:20][CH2:19][CH2:18][C:17](=[N:2][OH:3])[C:16]=2[CH:23]=1
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참가 물질

6

반응물 3

HCID 10340Sodium CarbonateHCID 443297Hydroxyamine hydrochlorideHCID 135224797-METHOXY-2,3,4,5-TETRAHYDRO-1-BENZOXEPIN-5-ONE

생성물 1

HCID 858439917-Methoxy-3,4-dihydro-1-benzoxepin-5-one oxime

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매2회

실험 절차

6.95 g of hydroxylamine hydrochloride dissolved in 15 ml of water and 5.3 g of sodium carbonate are added to a solution of 19.2 g of 7-methoxy-3,4-dihydro-1-benzoxepin-5-one in 45 ml of ethanol. The mixture is left at room temperature for 24 hours with stirring. 100 ml of water are then added and the alcohol is evaporated. The aqueous solution is make alkaline by the addition of soda and unreacted benzoxepin is extracted with ether. The aqueous phase is neutralised and the desired oxime is extracted with ether. After drying of the organic solution and evaporation of the solvent under reduced pressure, a white solid is obtained which, when recrystallised from cyclohexane yields 17 g of the desired pure product which has a melting point of 103° to 104° C.

후처리

  1. customthe alcohol is evaporated
  2. additionby the addition of soda and unreacted benzoxepin
  3. extractionis extracted with ether
  4. extractionthe desired oxime is extracted with ether
  5. customAfter drying of the organic solution and evaporation of the solvent under reduced pressure
  6. customa white solid is obtained which, when
  7. customrecrystallised from cyclohexane
  8. customyields 17 g of the desired pure product which

출처 및 근거

ORD 기록
ord-9b4b12e384c74b5285ea963e701d317f
출처 데이터셋
uspto-grants-1979_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04179516

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