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Potassium Iodide → Cyclohexanone, 2,2-dimethyl-6-(phenylmethylene)-

HRID 1377107
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HRID 1377107 반응식
[OH-].[K+].[I-].[K+].[CH3:5][CH:6]1[CH2:11][CH2:10][CH2:9][C:8](=[CH:12][C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)[C:7]1=[O:19].[CH3:20]Cl>C(O)(C)(C)C>[CH3:5][C:6]1([CH3:20])[CH2:11][CH2:10][CH2:9][C:8](=[CH:12][C:13]2[CH:14]=[CH:15][CH:16]=[CH:17][CH:18]=2)[C:7]1=[O:19]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 4875Potassium IodideHCID 6327Methyl ChlorideHCID 14797Potassium HydroxideHCID 977022-Methyl-6-(phenylmethylene)cyclohexanone

생성물 1

HCID 598624Cyclohexanone, 2,2-dimethyl-6-(phenylmethylene)-

시약·촉매·용매 1

HCID 6386tert-Butanol용매

실험 절차

66 g of 85% strength potassium hydroxide solution and 750 ml of tert-butanol were placed in a 1 l 4-necked flask, and the mixture was heated briefly at reflux with stirring. Then 8.3 g of potassium iodide were added, the mixture was cooled to room temperature and 200 g of 2-methyl-6-benzylidene-cyclohexanone were added. 101 g of methyl chloride were passed in at room temperature over 8 hours. The mixture was subsequently stirred at room temperature for 8 hours, and then 450 ml of tert-butanol were distilled off. 500 ml of water were added to the residue, the mixture was stirred thoroughly, and the product which separates out was filtered off with suction. Recrystallization from methanol gave 161 g (75% of theory) of pure product with a melting point of 79°-81° C.,

후처리

  1. temperaturethe mixture was heated briefly
  2. temperatureat reflux
  3. stirringThe mixture was subsequently stirred at room temperature for 8 hours
  4. distillation450 ml of tert-butanol were distilled off
  5. addition500 ml of water were added to the residue
  6. stirringthe mixture was stirred thoroughly
  7. filtrationthe product which separates out was filtered off with suction
  8. customRecrystallization from methanol
  9. customgave 161 g (75% of theory) of pure product with a melting point of 79°-81° C.

출처 및 근거

ORD 기록
ord-0a1324ce3e584f83b007e0c4c15f4a8e
출처 데이터셋
uspto-grants-1997_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05663447

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