Sodium Hydroxide → Desoxyanisoin Oxime

HRID 2286276

反応式

HRID 2286276 の反応式
[C:1]1([C:9]([CH2:11][C:12]2[CH:19]=[CH:18][C:15]([O:16][CH3:17])=[CH:14][CH:13]=2)=O)[CH:8]=[CH:7][C:4]([O:5][CH3:6])=[CH:3][CH:2]=1.Cl.[NH2:21][OH:22].[OH-].[Na+]>CO.O>[C:1]1([C:9](=[N:21][OH:22])[CH2:11][C:12]2[CH:19]=[CH:18][C:15]([O:16][CH3:17])=[CH:14][CH:13]=2)[CH:8]=[CH:7][C:4]([O:5][CH3:6])=[CH:3][CH:2]=1

参加物

6

反応物 3

HCID 14798Sodium HydroxideHCID 67120DesoxyanisoinHCID 443297Hydroxyamine hydrochloride

生成物 1

HCID 231097Desoxyanisoin Oxime収率 98.6%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒2 回HCID 962Water溶媒

実験手順

Desoxyanisoin (98%, 52.2 g., 0.2 mole) and hydroxylamine hydrochloride (15.3 g., 0.22 mole) are slurried in a mixture of methanol (300 ml) and water (200 ml) and sodium hydroxide (16 g., 0.4 mole) is added slowly. The mixture is stirred for 15 minutes, then placed in a hot water bath (70° C.) and stirred an additional hour. Methanol is then added to the hot mixture until solution is almost complete, the mixture is filtered and concentrated to remove most of the methanol, then cooled with the addition of ice-water. Filtered, dissolved the resulting solid in ethyl acetate, extracted with brine. Dried the organic layer (Na2SO4), filtered and concentrated to obtain 53.5 g (98.5%) of the oxime as a yellow solid.

後処理

  1. additionis added slowly
  2. customplaced in a hot water bath
  3. stirring(70° C.) and stirred an additional hour
  4. filtrationthe mixture is filtered
  5. concentrationconcentrated
  6. customto remove most of the methanol
  7. temperaturecooled with the addition of ice-water
  8. filtrationFiltered
  9. dissolutiondissolved the resulting solid in ethyl acetate
  10. extractionextracted with brine
  11. dry with materialDried the organic layer (Na2SO4)
  12. filtrationfiltered
  13. concentrationconcentrated

出典と根拠

ORDレコード
ord-ebe1373d01a44967b359eaa67873688b
出典データセット
uspto-grants-1982_04
特許番号
US04327222

関連ノート

読み込み中…