2,3,4,5-Tetrahydro-1-benzoxepin-5-one → 3,4-dihydro-1-benzoxepin-5(2H)-one oxime

HRID 2271074

反応式

HRID 2271074 の反応式
[O:1]1[C:7]2[CH:8]=[CH:9][CH:10]=[CH:11][C:6]=2[C:5](=O)[CH2:4][CH2:3][CH2:2]1.Cl.[NH2:14][OH:15]>C(O)C.N1C=CC=CC=1>[O:1]1[C:7]2[CH:8]=[CH:9][CH:10]=[CH:11][C:6]=2[C:5](=[N:14][OH:15])[CH2:4][CH2:3][CH2:2]1

参加物

5

反応物 2

HCID 3155752,3,4,5-Tetrahydro-1-benzoxepin-5-oneHCID 443297Hydroxyamine hydrochloride

生成物 1

HCID 732003533,4-dihydro-1-benzoxepin-5(2H)-one oxime収率 92.8%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 1049Pyridine溶媒

実験手順

A solution of 10.0 g (62 mmol) of 3,4-dihydro-1-benzoxepin-5(2H)-one (J. Chem. Soc., Perkin Trans. 1 (1991), 2763) and 4.63 g (68 mmol) of hydroxylamine hydrochloride in 45 ml of ethanol and 45 ml of pyridine was heated under reflux for 5 h. After distilling off the solvents on a rotary evaporator, the residue was treated with water, adjusted to pH 2 with dil. hydrochloric acid and stirred for 3 h. After filtering off the precipitated product with suction and drying it, 10.2 g of 3,4-dihydro-1-benzoxepin-5(2H)-one oxime were obtained, m.p. 96-98° C.

後処理

  1. temperatureunder reflux for 5 h
  2. distillationAfter distilling off the solvents
  3. customon a rotary evaporator
  4. additionthe residue was treated with water
  5. filtrationAfter filtering off the precipitated product with suction
  6. customdrying it

出典と根拠

ORDレコード
ord-088a30e1f5564441806dd06c265ab31f
出典データセット
uspto-grants-2001_12
特許番号
US06333349B1

関連ノート

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