Sodium Hydroxide → 2-[3-(Hydroxyimino)butyl]-1H-isoindole-1,3(2H)-dione

HRID 248763

反応式

HRID 248763 の反応式
O=[C:2]([CH3:16])[CH2:3][CH2:4][N:5]1[C:9](=[O:10])[C:8]2=[CH:11][CH:12]=[CH:13][CH:14]=[C:7]2[C:6]1=[O:15].Cl.[NH2:18][OH:19].[OH-].[Na+].C(=O)([O-])O.[Na+]>CO>[OH:19][N:18]=[C:2]([CH3:16])[CH2:3][CH2:4][N:5]1[C:9](=[O:10])[C:8]2=[CH:11][CH:12]=[CH:13][CH:14]=[C:7]2[C:6]1=[O:15]

参加物

6

反応物 4

HCID 14798Sodium HydroxideHCID 2907282-(3-Oxobutyl)isoindoline-1,3-dioneHCID 443297Hydroxyamine hydrochlorideHCID 516892Sodium Bicarbonate

生成物 1

HCID 714040032-[3-(Hydroxyimino)butyl]-1H-isoindole-1,3(2H)-dione収率 84.4%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

1.08 g (5.00 mmol) of N-(3-oxobutyl)phthalimide was dissolved in 10 ml of methanol and to the solution was added 0.695 g (10.0 mmol) of hydroxylamine hydrochloride. To this suspension was added 2 ml of 5N aqueous sodium hydroxide solution, followed by being stirred at room temperature for 16 hours. The reaction mixture was poured into 100 ml of saturated aqueous sodium hydrogencarbonate and extracted with chloroform (30 ml×3), and the combined organic layer was dried over magnesium sulfate. Chloroform was distilled off and the residual solids were washed with hexane to give 0.98 g (yield 84%) of the titled compound as colorless crystals.

後処理

  1. extractionextracted with chloroform (30 ml×3)
  2. dry with materialthe combined organic layer was dried over magnesium sulfate
  3. distillationChloroform was distilled off
  4. washthe residual solids were washed with hexane

出典と根拠

ORDレコード
ord-f0c45504eaf34f9caf46112495a7d00c
出典データセット
uspto-grants-1993_05
特許番号
US05211738

関連ノート

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