Ethyl trifluoroacetate → 4,4,4-Trifluoro-1-(4-fluorophenyl)butane-1,3-dione

HRID 1521118노트

반응식

HRID 1521118 반응식
[F:1][C:2]([F:9])([F:8])[C:3]([O:5]CC)=O.C[O-].[Na+].[CH3:13][C:14]([C:16]1[CH:21]=[CH:20][C:19]([F:22])=[CH:18][CH:17]=1)=[O:15]>C(OC)(C)(C)C.Cl>[F:9][C:2]([F:1])([F:8])[C:3](=[O:5])[CH2:13][C:14]([C:16]1[CH:21]=[CH:20][C:19]([F:22])=[CH:18][CH:17]=1)=[O:15]

참가 물질

6

반응물 3

HCID 9794Ethyl trifluoroacetateHCID 98284'-FluoroacetophenoneHCID 10942334Sodium Methoxide

생성물 1

HCID 27714764,4,4-Trifluoro-1-(4-fluorophenyl)butane-1,3-dione수율 97%

시약·촉매·용매 2

HCID 313Hydrochloric Acid용매HCID 15413tert-Butyl methyl ether용매

실험 절차

To a solution of ethyl trifluoroacetate (23.9 mL, 199 mmol) in tertbutylmethylether (230 mL) containing sodium methoxide (5.4 M, 39.6 mL, 214 mmol) was added 4-fluoroacetophenone (25 g, 181 mmol) and the resulting mixture stirred at room temperature for 3 h and then poured into ice-water. The mixture was then diluted with HCl (2 N, 200 mL) and then extracted with ethyl acetate. The combined organic extracts were then dried over sodium sulfate and evaporated to afford the title compound (40.9 g, 97%) which was obtained as an orange oil. MS: m/e=232.9 [M−H]−.

후처리

  1. extractionextracted with ethyl acetate
  2. dry with materialThe combined organic extracts were then dried over sodium sulfate
  3. customevaporated

출처 및 근거

ORD 기록
ord-3799f1658af44c68a3d03ee18e27fb72
출처 데이터셋
uspto-grants-2015_07
특허 번호
US09073908B2

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