HCID 67254019、化合物 → Methyl 4-methyl-5-(2-(trifluoromethyl)phenyl)-1H-pyrrole-3-carboxylate

HRID 912579ノート

反応式

HRID 912579 の反応式
[CH3:1][O:2][C:3]([CH:5]1[C:9]([CH3:10])=[C:8]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=2[C:17]([F:20])([F:19])[F:18])[NH:7][CH2:6]1)=[O:4]>C1(C)C=CC=CC=1.[Pd]>[CH3:1][O:2][C:3]([C:5]1[C:9]([CH3:10])=[C:8]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=2[C:17]([F:20])([F:19])[F:18])[NH:7][CH:6]=1)=[O:4]

参加物

4

反応物 1

HCID 67254019HCID 67254019、化合物

生成物 1

HCID 67251895Methyl 4-methyl-5-(2-(trifluoromethyl)phenyl)-1H-pyrrole-3-carboxylate収率 29.3%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 1140Toluene溶媒

実験手順

To a solution of 4-methyl-5-(2-trifluoromethyl-phenyl)-2,3-dihydro-1H-pyrrole-3-carboxylic acid methyl ester (10 g, 35 mmol) in toluene was added 10% Pd/C (3.3 g). The resulting suspension was heated to reflux for 3 days. After cooling, the solids were removed by filtration. The filtrate was washed with toluene and concentrated under reduced pressure to yield an oil, which was purified by column chromatography (silica), eluting with EtOAc-hexane (1:1) to give the title compound (2.9 g, 29%). MS (ES): 284 (MH+).

後処理

  1. temperatureThe resulting suspension was heated
  2. temperatureto reflux for 3 days
  3. temperatureAfter cooling
  4. customthe solids were removed by filtration
  5. washThe filtrate was washed with toluene
  6. concentrationconcentrated under reduced pressure
  7. customto yield an oil, which
  8. customwas purified by column chromatography (silica)
  9. washeluting with EtOAc-hexane (1:1)

出典と根拠

ORDレコード
ord-3eb8825f49d644e588555b10246ce8c4
出典データセット
uspto-grants-2011_09
特許番号
US08026237B2

反応ノート

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