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

HRID 1521118ノート

反応式

HRID 1521118 の反応式
[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]

参加物

6

反応物 3

HCID 9794Ethyl trifluoroacetateHCID 98284'-FluoroacetophenoneHCID 10942334Sodium Methoxide

生成物 1

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

試薬・触媒・溶媒 2

HCID 313Hydrochloric Acid溶媒HCID 15413tert-Butyl methyl ether溶媒

実験手順

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]−.

後処理

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

出典と根拠

ORDレコード
ord-3799f1658af44c68a3d03ee18e27fb72
出典データセット
uspto-grants-2015_07
特許番号
US09073908B2

反応ノート

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