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

HRID 1448062
ノート
印刷プレビュー

反応式

HRID 1448062 の反応式
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
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒2 回

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-9b4b12e384c74b5285ea963e701d317f
出典データセット
uspto-grants-1979_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04179516

反応ノート

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