Sodium Hydroxide → 1,2,2,6,6-Pentamethyl-piperidin-4-one oxime

HRID 1070699

反応式

HRID 1070699 の反応式
I.[CH3:2][N:3]1[C:8]([CH3:10])([CH3:9])[CH2:7][C:6](=O)[CH2:5][C:4]1([CH3:13])[CH3:12].Cl.[NH2:15][OH:16].[OH-].[Na+]>O>[CH3:2][N:3]1[C:8]([CH3:10])([CH3:9])[CH2:7][C:6](=[N:15][OH:16])[CH2:5][C:4]1([CH3:13])[CH3:12]

参加物

5

反応物 3

HCID 14798Sodium HydroxideHCID 443297Hydroxyamine hydrochlorideHCID 223975731,2,2,6,6-Pentamethyl-4-piperidone hydroiodide

生成物 1

HCID 2419501,2,2,6,6-Pentamethyl-piperidin-4-one oxime収率 83.3%

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

実験手順

A suspension of 1,2,2,6,6-pentamethyl-4-piperidone hydroiodide (3 g, 10.1 mmol) and hydroxylamine hydrochloride (980 mg, 14 mmol) in water (6 ml) was stirred at RT for 15 minutes. Solid NaOH was added until basic pH and thickening of the suspension. Water (3 ml) was added and stirring at RT was continued overnight. The suspension was filtered and the solid washed with water (few ml) and dried. The solid was then dissolved in Et2O, the solution was dried (MgSO4) and concentrated to give after drying pure title compound (1.55 g, 8.41 mmol, yield 83.3%) as white crystals.

後処理

  1. stirringstirring at RT
  2. waitwas continued overnight
  3. filtrationThe suspension was filtered
  4. washthe solid washed with water (few ml)
  5. customdried
  6. dissolutionThe solid was then dissolved in Et2O
  7. dry with materialthe solution was dried (MgSO4)
  8. concentrationconcentrated
  9. customto give

出典と根拠

ORDレコード
ord-20f3f91506e544d7a8f2cfe8052b4ca4
出典データセット
uspto-grants-2005_06
特許番号
US06903117B2

関連ノート

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