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Potassium Carbonate → 2-Methyl-4-(2,5-dimethylphenyl)thio-2-butene

HRID 368932
ノート
印刷プレビュー

反応式

HRID 368932 の反応式
Br[CH2:2][CH:3]=[C:4]([CH3:6])[CH3:5].C(=O)([O-])[O-].[K+].[K+].[CH3:13][C:14]1[CH:19]=[CH:18][C:17]([CH3:20])=[CH:16][C:15]=1[SH:21]>CC(C)=O>[CH3:5][C:4](=[CH:3][CH2:2][S:21][C:15]1[CH:16]=[C:17]([CH3:20])[CH:18]=[CH:19][C:14]=1[CH3:13])[CH3:6]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 700922-Butene, 1-bromo-3-methyl-HCID 776152,5-Xylenethiol

生成物 1

HCID 129936832-Methyl-4-(2,5-dimethylphenyl)thio-2-butene収率 100.3%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

80 ml of acetone, 9.1 g (0.06 mol) of 1-bromo-3-methyl-2-butene and 8.0 g (0.058 mol) of anhydrous potassium carbonate were added to 8.0 g (0.058 mol) of 2,5-dimethyl-thiophenol, and the mixture was refluxed under heat for 1 hour. After the completion of the reaction, a formed salt was removed by filtration, and the acetone was distilled off under reduced pressure. Then, ethyl acetate was added to the residue, and the mixture was washed with a saturated sodium chloride aqueous solution. The mixture was dried over anhydrous sodium sulfate, and then the ethyl acetate was distilled off to give 12 g (yield 100%) of 2-methyl-4-(2,5-dimethylphenyl)thio-2-butene.

後処理

  1. temperaturethe mixture was refluxed
  2. temperatureunder heat for 1 hour
  3. customAfter the completion of the reaction
  4. customa formed salt was removed by filtration
  5. distillationthe acetone was distilled off under reduced pressure
  6. additionThen, ethyl acetate was added to the residue
  7. washthe mixture was washed with a saturated sodium chloride aqueous solution
  8. dry with materialThe mixture was dried over anhydrous sodium sulfate
  9. distillationthe ethyl acetate was distilled off

出典と根拠

ORDレコード
ord-09852a2aff6d4745afe727db2d477c94
出典データセット
uspto-grants-2000_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06136755

反応ノート

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