Hydroxyamine hydrochloride → 5,7-Dimethyl-8-hydroxy-1,2,3,4,4a,9a-hexahydro-9-fluorenone oxime

HRID 2051426ノート

反応式

HRID 2051426 の反応式
Cl.[NH2:2][OH:3].[CH3:4][C:5]1[CH:17]=[C:16]([CH3:18])[C:15]([OH:19])=[C:14]2[C:6]=1[CH:7]1[CH:12]([C:13]2=O)[CH2:11][CH2:10][CH2:9][CH2:8]1>N1C=CC=CC=1>[CH3:4][C:5]1[CH:17]=[C:16]([CH3:18])[C:15]([OH:19])=[C:14]2[C:6]=1[CH:7]1[CH:12]([C:13]2=[N:2][OH:3])[CH2:11][CH2:10][CH2:9][CH2:8]1

参加物

4

反応物 2

HCID 443297Hydroxyamine hydrochlorideHCID 151571835,7-Dimethyl-8-hydroxy-1,2,3,4,4a,9a-hexahydro-9-fluorenone

生成物 1

HCID 1363411795,7-Dimethyl-8-hydroxy-1,2,3,4,4a,9a-hexahydro-9-fluorenone oxime

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

7.99 Grams of hydroxylamine hydrochloride was added to a solution prepared by dissolving 17.22 g of 5,7-dimethyl-8-hydroxy-1,2,3,4,4a,9a-hexahydro-9-fluorenone in 100 ml of pyridine and the mixture was refluxed under heating for 2 hours. Pyridine was distilled off under reduced pressure and the resulting residue was extracted with 300 ml of chloroform. The extract was washed with water 1% hydrochloric acid and then with saturated aqueous sodium chloride solution and then dried with anhydrous magnesium sulfate. After the solvent was distilled off, the product was recrystallized from ethanol to obtain 11.56 g of 5,7-dimethyl-8-hydroxy-1,2,3,4,4a,9a-hexahydro-9-fluorenone oxime as a mixture of syn-isomer and anti-isomer.

後処理

  1. customprepared
  2. temperaturethe mixture was refluxed
  3. temperatureunder heating for 2 hours
  4. distillationPyridine was distilled off under reduced pressure
  5. extractionthe resulting residue was extracted with 300 ml of chloroform
  6. washThe extract was washed with water 1% hydrochloric acid
  7. dry with materialwith saturated aqueous sodium chloride solution and then dried with anhydrous magnesium sulfate
  8. distillationAfter the solvent was distilled off
  9. customthe product was recrystallized from ethanol

出典と根拠

ORDレコード
ord-1a708f3666034e64bbe548a4cc770e5f
出典データセット
uspto-grants-1991_05
特許番号
US05017724

反応ノート

読み込み中…