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

HRID 6693

반응식

HRID 6693 반응식
[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]

참가 물질

7

반응물 5

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

생성물 1

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

시약·촉매·용매 1

HCID 15413tert-Butyl methyl ether용매

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-697eb1beb35a4059a73112f3071f16a1
출처 데이터셋
uspto-grants-2006_08
특허 번호
US07084148B2

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