Potassium Carbonate → 2-(3-Methyl-4-nitro-phenyl)-thioacetimidic acid 3,3,4,4,4-pentafluoro-2-oxo-butyl ester

HRID 2243278ノート

反応式

HRID 2243278 の反応式
[CH3:1][C:2]1[CH:3]=[C:4]([CH2:11][C:12]([NH2:14])=[S:13])[CH:5]=[CH:6][C:7]=1[N+:8]([O-:10])=[O:9].Br[CH2:16][C:17](=[O:25])[C:18]([F:24])([F:23])[C:19]([F:22])([F:21])[F:20].C(=O)([O-])[O-].[K+].[K+]>CN(C=O)C.C(OCC)(=O)C>[F:23][C:18]([F:24])([C:19]([F:22])([F:21])[F:20])[C:17](=[O:25])[CH2:16][S:13][C:12](=[NH:14])[CH2:11][C:4]1[CH:5]=[CH:6][C:7]([N+:8]([O-:10])=[O:9])=[C:2]([CH3:1])[CH:3]=1

参加物

6

反応物 3

HCID 11430Potassium CarbonateHCID 27363551-Bromo-3,3,4,4,4-pentafluorobutan-2-oneHCID 592103882-(3-Methyl-4-nitrophenyl)ethanethioamide

生成物 1

HCID 866171452-(3-Methyl-4-nitro-phenyl)-thioacetimidic acid 3,3,4,4,4-pentafluoro-2-oxo-butyl ester収率 73.8%

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

実験手順

2-(3-Methyl-4-nitrophenyl)-thioacetamide (1.00 g), 1-bromo-3,3,4,4,4-pentafluoro-2-butanone (1.15 g) and potassium carbonate (0.79 g) were stirred in DMF (10 ml) at room temperature for 1 hour. The reaction solution was diluted with ethyl acetate and washed with water and saturated aqueous solution of sodium chloride. After drying the organic layer with magnesium sulfate, the solvent was distilled off under the reduced pressure and the obtained residue was purified by silica gel column chromatography to obtain 2-(3-Methyl-4-nitro-phenyl)-thioacetimidic acid 3,3,4,4,4-pentafluoro-2-oxo-butyl ester (1.30 g).

後処理

  1. washwashed with water and saturated aqueous solution of sodium chloride
  2. dry with materialAfter drying the organic layer with magnesium sulfate
  3. distillationthe solvent was distilled off under the reduced pressure
  4. customthe obtained residue was purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-e9c198d0a42f4eb79d55f7f0f2487208
出典データセット
uspto-grants-2010_03
特許番号
US07674807B2

反応ノート

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