Hydroxyamine hydrochloride → 5-n-Butylindan-1-one oxime

HRID 19716ノート

反応式

HRID 19716 の反応式
Cl.[NH2:2][OH:3].C([O-])(=O)C.[Na+].[CH2:9]([C:13]1[CH:14]=[C:15]2[C:19](=[CH:20][CH:21]=1)[C:18](=O)[CH2:17][CH2:16]2)[CH2:10][CH2:11][CH3:12]>C(O)C.O>[CH2:9]([C:13]1[CH:14]=[C:15]2[C:19](=[CH:20][CH:21]=1)[C:18](=[N:2][OH:3])[CH2:17][CH2:16]2)[CH2:10][CH2:11][CH3:12]

参加物

6

反応物 3

HCID 443297Hydroxyamine hydrochlorideHCID 517045Sodium AcetateHCID 149399645-n-Butylindan-1-one

生成物 1

HCID 860040385-n-Butylindan-1-one oxime

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒2 回

実験手順

Hydroxylamine hydrochloride (0.89 g, 12.8 mmol) and sodium acetate (12.8 mmol) are added to a solution of 5-n-butylindan-1-one (1.0 g, 5.31 mmol) in ethanol (30 ml) and water (3 ml). The reaction is heated to reflux for 20 minutes, then water is added and the mixture is extracted with CH2Cl2. The combined organic extracts are washed with brine, dried (MgSO4) and evaporated to afford the title compound. NMR δH 0.86 (t J 7.3 3H), 1.28 (sextet J 7.3 2H), 1.52 (quintet J 7.3 2H), 2.55 (t J 8.0 2H), 2.85-3.0 (m 4H), 7.0 (d J 8.3 1H), 7.05 (s 1H), 7.45 (d J 8.3 2H)

後処理

  1. temperatureThe reaction is heated
  2. temperatureto reflux for 20 minutes
  3. extractionthe mixture is extracted with CH2Cl2
  4. washThe combined organic extracts are washed with brine
  5. dry with materialdried (MgSO4)
  6. customevaporated

出典と根拠

ORDレコード
ord-f90580b923b54dcea6cf2698b7828a3e
出典データセット
uspto-grants-2010_06
特許番号
US07745462B2

反応ノート

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