Sodium Hydroxide → Desoxyanisoin Oxime

HRID 2286276

반응식

HRID 2286276 반응식
[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

참가 물질

6

반응물 3

HCID 14798Sodium HydroxideHCID 67120DesoxyanisoinHCID 443297Hydroxyamine hydrochloride

생성물 1

HCID 231097Desoxyanisoin Oxime수율 98.6%

시약·촉매·용매 2

HCID 887Methanol용매2회HCID 962Water용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-ebe1373d01a44967b359eaa67873688b
출처 데이터셋
uspto-grants-1982_04
특허 번호
US04327222

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