Sodium Hydroxide → 2-Hydroxy-2-methyl-1-[4-(methylthio)phenyl]-1-butanone

HRID 367363

反応式

HRID 367363 の反応式
[CH3:1][CH:2]([CH2:13][CH3:14])[C:3]([C:5]1[CH:10]=[CH:9][C:8]([S:11][CH3:12])=[CH:7][CH:6]=1)=[O:4].[OH-:15].[Na+]>C1(C)C=CC=CC=1.C(Cl)(Cl)(Cl)Cl.Cl.[NH4+].[Cl-]>[OH:15][C:2]([CH3:1])([CH2:13][CH3:14])[C:3]([C:5]1[CH:6]=[CH:7][C:8]([S:11][CH3:12])=[CH:9][CH:10]=1)=[O:4]

参加物

7

反応物 2

HCID 14798Sodium HydroxideHCID 154806432-Methyl-1-[4-(methylthio)phenyl]-1-butanone

生成物 1

HCID 101307312-Hydroxy-2-methyl-1-[4-(methylthio)phenyl]-1-butanone

試薬・触媒・溶媒 4

HCID 313Hydrochloric Acid溶媒HCID 1140Toluene溶媒HCID 5943Carbon Tetrachloride溶媒HCID 25517Ammonium Chloride溶媒

実験手順

To a solution of the ketone from step 1 (33 g) in toluene (48 mL), CCl4 (23.5 mL) and Aliquat, 336 (10.5 mL), was added NaOH pellets (14.5 g) and the resulting mixture was vigorously stirred for 2 days. The reaction mixture was diluted with 5N HCl, aqueous NH4Cl and extracted with Et2O. The organic layer was dried over Na2SO4 and concentrated. The crude product was purified by flash chromatography eluted with EtOAc/Hexane 9% to give a yellow syrup.

後処理

  1. extractionextracted with Et2O
  2. dry with materialThe organic layer was dried over Na2SO4
  3. concentrationconcentrated
  4. customThe crude product was purified by flash chromatography
  5. washeluted with EtOAc/Hexane 9%
  6. customto give a yellow syrup

出典と根拠

ORDレコード
ord-311f7a1abbbf468b94f4f1a55dd01342
出典データセット
uspto-grants-2000_10
特許番号
US06133292

関連ノート

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