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

HRID 1377107
ノート
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反応式

HRID 1377107 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6386tert-Butanol溶媒

実験手順

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.,

後処理

  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.

出典と根拠

ORDレコード
ord-0a1324ce3e584f83b007e0c4c15f4a8e
出典データセット
uspto-grants-1997_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05663447

反応ノート

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