Hydrochloric Acid → 1,3-Butanedione, 4,4,4-trifluoro-1-[4-(methylthio)phenyl]-

HRID 6693

反応式

HRID 6693 の反応式
[F:1][C:2]([F:9])([F:8])[C:3]([O:5]CC)=O.C[O-].[Na+].CO.[CH3:15][C:16]([C:18]1[CH:23]=[CH:22][C:21]([S:24][CH3:25])=[CH:20][CH:19]=1)=[O:17].Cl>CC(OC)(C)C>[F:9][C:2]([F:1])([F:8])[C:3](=[O:5])[CH2:15][C:16]([C:18]1[CH:23]=[CH:22][C:21]([S:24][CH3:25])=[CH:20][CH:19]=1)=[O:17]

参加物

7

反応物 5

HCID 313Hydrochloric AcidHCID 887MethanolHCID 9794Ethyl trifluoroacetateHCID 745011-(4-(Methylthio)phenyl)ethan-1-oneHCID 10942334Sodium Methoxide

生成物 1

HCID 107301701,3-Butanedione, 4,4,4-trifluoro-1-[4-(methylthio)phenyl]-収率 71%

試薬・触媒・溶媒 1

HCID 15413tert-Butyl methyl ether溶媒

実験手順

To a solution of ethyl trifluoroacetate (7.95 ml, 1.1 eq) in MTBE (125 ml) was added dropwise 25% sodium methoxide in methanol (16 ml, 1.2 eq). 4-Methylthioacetophenone (Aldrich, 10 g, 0.06 mol) was added portionwise and the mixture stirred at ambient temperature overnight. 2N Hydrochloric acid (40 ml) was added cautiously and the organic phase separated, washed with brine and dried (Na2SO4) to give an orange solid. The orange solid was recrystallised from hot isopropanol to give the title compound as a yellow crystalline solid (11.25 g, 71%).

後処理

  1. customthe organic phase separated
  2. washwashed with brine
  3. dry with materialdried (Na2SO4)
  4. customto give an orange solid
  5. customThe orange solid was recrystallised from hot isopropanol

出典と根拠

ORDレコード
ord-697eb1beb35a4059a73112f3071f16a1
出典データセット
uspto-grants-2006_08
特許番号
US07084148B2

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