Potassium Hydroxide → 2-Hydroxy-4,4,6,6-tetramethylcyclohex-2-en-1-one

HRID 1758013노트

반응식

HRID 1758013 반응식
[OH-:1].[K+].Br[CH:4]1[C:9]([CH3:11])([CH3:10])[CH2:8][C:7]([CH3:13])([CH3:12])[CH:6](Br)[C:5]1=[O:15]>O>[OH:15][C:5]1[C:6](=[O:1])[C:7]([CH3:13])([CH3:12])[CH2:8][C:9]([CH3:11])([CH3:10])[CH:4]=1

참가 물질

4

반응물 2

HCID 14797Potassium HydroxideHCID 1027432,6-Dibromo-3,3,5,5-tetramethylcyclohexan-1-one

생성물 1

HCID 5741832-Hydroxy-4,4,6,6-tetramethylcyclohex-2-en-1-one

시약·촉매·용매 1

HCID 962Water용매

실험 절차

To a stirred solution of potassium hydroxide (50 g) in 1500 ml of distilled water was added the brominated compound of step 1 (50 g). Stirring was continued for 24 hours. The solution was filtered to remove brominated compound which had not dissolved. The filtrate was cooled in an ice bath and concentrated sulphuric acid added dropwise until a white solid precipitated. The mixture was stirred for 30 minutes, after which the white solid was collected and recrystallized from a hot mixture of 200 ml of methanol and 100 ml of water, giving 2-hydroxy-4,4,6,6-tetramethylcyclohex-2-enone as white crystals, 13.5 g, melting range 85°-86° C.

후처리

  1. filtrationThe solution was filtered
  2. customto remove brominated compound which
  3. dissolutionhad not dissolved
  4. temperatureThe filtrate was cooled in an ice bath
  5. additionconcentrated sulphuric acid added dropwise until a white solid
  6. customprecipitated
  7. stirringThe mixture was stirred for 30 minutes
  8. customafter which the white solid was collected
  9. customrecrystallized from a hot mixture of 200 ml of methanol and 100 ml of water

출처 및 근거

ORD 기록
ord-174aa176362846b5a416204e57d67433
출처 데이터셋
uspto-grants-1983_02
특허 번호
US04371603

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