p-Toluenesulfonic acid → HCID 57001829、化合物

HRID 2249098ノート

反応式

HRID 2249098 の反応式
[F:1][C:2]1[CH:7]=[CH:6][C:5]([S:8][CH2:9][CH:10]([CH3:17])[CH:11](O)[CH2:12][C:13](=[O:15])[CH3:14])=[CH:4][CH:3]=1.C1(C)C=CC(S(O)(=O)=O)=CC=1>C1(C)C=CC=CC=1>[F:1][C:2]1[CH:3]=[CH:4][C:5]([S:8][CH2:9][CH:10]([CH3:17])[CH:11]=[CH:12][C:13](=[O:15])[CH3:14])=[CH:6][CH:7]=1

参加物

4

反応物 2

HCID 6101p-Toluenesulfonic acidHCID 146928186-(4-Fluorophenylthio)-4-hydroxy-5-methyl-2-hexanone

生成物 1

HCID 57001829HCID 57001829、化合物収率 96.8%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

1.00 Gram of 6-(4-fluorophenylthio)-4-hydroxy-5-methyl-2-hexanone was dissolved in 100 ml of toluene, and 0.02 g of p-toluene sulfonic acid was added thereto. The resulting mixture was refluxed for 1.5 hours with stirring. After having been cooled, the mixture was washed with a saturated aqueous sodium hydrogencarbonate solution and then saturated aqueous sodium chloride solution. Then the mixture was dried over anhydrous magnesium sulfate. Removing the solvent from the mixture under reduced pressure gave 1.08 g of 6-(4-fluorophenylthio)-5-methyl-3-hexen-2-one. (trans : cis =3.7 : 1) (purity: 83.5%). The yield was 96.8%. Production example 61

後処理

  1. temperatureThe resulting mixture was refluxed for 1.5 hours
  2. temperatureAfter having been cooled
  3. washthe mixture was washed with a saturated aqueous sodium hydrogencarbonate solution
  4. dry with materialThen the mixture was dried over anhydrous magnesium sulfate
  5. customRemoving the solvent from the mixture under reduced pressure

出典と根拠

ORDレコード
ord-49529812af7d44a8a2358220433b2e0b
出典データセット
uspto-grants-1991_08
特許番号
US05041679

反応ノート

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