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Hydrochloric Acid → 1-(3,4-Dimethoxyphenyl)-4,4,4-trifluorobutane-1,3-dione

HRID 2210635
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HRID 2210635 반응식
C[O-].[Na+].[F:4][C:5]([F:12])([F:11])[C:6]([O:8]CC)=O.[CH3:13][C:14]([C:16]1[CH:21]=[CH:20][C:19]([O:22][CH3:23])=[C:18]([O:24][CH3:25])[CH:17]=1)=[O:15].Cl>C1(C)C=CC=CC=1.O>[CH3:25][O:24][C:18]1[CH:17]=[C:16]([C:14](=[O:15])[CH2:13][C:6](=[O:8])[C:5]([F:4])([F:11])[F:12])[CH:21]=[CH:20][C:19]=1[O:22][CH3:23]
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참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 9794Ethyl trifluoroacetateHCID 143283,4-Dimethoxyphenyl methyl ketoneHCID 10942334Sodium Methoxide

생성물 1

HCID 69172031-(3,4-Dimethoxyphenyl)-4,4,4-trifluorobutane-1,3-dione수율 96%

시약·촉매·용매 2

HCID 962Water
용매
HCID 1140Toluene용매2회

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온도
50 °C

실험 절차

216 g (4 mol) of anhydrous sodium methylate and 3.5 l of toluene are introduced into a 10 liter round-bottomed flask and, under vigorous stirring, 705 g (5 mol) of ethyl trifluoroacetate are then run in; the temperature rises slowly to 30° C. After cooling in an ice bath, a solution of 720 g (4 mol) of 3,4-dimethoxyacetophenone in 0.5 l of toluene is added dropwise to the reaction mixture; a white precipitate slowly forms. The mixture is next left stirred overnight and then heated to 50° C. for three hours. After cooling, 2 1 of water and 330 ml of concentrated hydrochloric acid are added, the organic phase is separated off after settling has taken place, dried over magnesium sulphate, filtered and evaporated to obtain 1060 g (96%) of a yellow solid melting at 87°-89° C.

후처리

  1. customrises slowly to 30° C
  2. temperatureAfter cooling in an ice bath
  3. waitThe mixture is next left
  4. temperatureAfter cooling
  5. customthe organic phase is separated off after settling
  6. dry with materialdried over magnesium sulphate
  7. filtrationfiltered
  8. customevaporated

출처 및 근거

ORD 기록
ord-ced4b3146bce44aeb88c5de9966e7e24
출처 데이터셋
uspto-grants-1995_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05459262

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