Potassium Carbonate → 4-iodo-1-(3-methyl-4-nitrobenzyl)-2-trifluoroacetyl-1H-pyrrole

HRID 2243261ノート

反応式

HRID 2243261 の反応式
[CH3:1][C:2]1[CH:3]=[C:4]([CH:7]=[CH:8][C:9]=1[N+:10]([O-:12])=[O:11])[CH2:5]Cl.[I:13][C:14]1[CH:15]=[C:16]([C:19](=[O:24])[C:20]([F:23])([F:22])[F:21])[NH:17][CH:18]=1.C(=O)([O-])[O-].[K+].[K+]>CN(C=O)C.C(OCC)(=O)C>[I:13][C:14]1[CH:15]=[C:16]([C:19](=[O:24])[C:20]([F:21])([F:22])[F:23])[N:17]([CH2:5][C:4]2[CH:7]=[CH:8][C:9]([N+:10]([O-:12])=[O:11])=[C:2]([CH3:1])[CH:3]=2)[CH:18]=1

参加物

6

反応物 3

HCID 11430Potassium CarbonateHCID 87687Alpha-chloro-3-methyl-4-nitrotolueneHCID 592104064-Iodo-2-(trifluoroacetyl)pyrrole

生成物 1

HCID 592104184-iodo-1-(3-methyl-4-nitrobenzyl)-2-trifluoroacetyl-1H-pyrrole収率 33.4%

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

実験手順

3-Methyl-4-nitrobenzyl chloride (0.63 g), 4-iodo-2-(trifluoroacetyl)pyrrole (0.89 g) and potassium carbonate (0.57 g) were stirred in DMF (10 ml) at room temperature for 2 hours. 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 4-iodo-1-(3-methyl-4-nitrobenzyl)-2-trifluoroacetyl-1H-pyrrole (0.45 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-70eac498f4c749a4940a15493d4aa70f
出典データセット
uspto-grants-2010_03
特許番号
US07674807B2

反応ノート

読み込み中…