Ethanol → HCID 178471163、化合物

HRID 349942ノート

反応式

HRID 349942 の反応式
C([N:8]1[CH:12]=[C:11]([CH2:13][CH2:14][C:15]([O:17][CH2:18][CH3:19])=[O:16])[C:10]([O:20][CH2:21][CH3:22])=[N:9]1)C1C=CC=CC=1.C(O)C>[C].[Pd].C(O)=O>[CH2:21]([O:20][C:10]1[C:11]([CH2:13][CH2:14][C:15]([O:17][CH2:18][CH3:19])=[O:16])=[CH:12][NH:8][N:9]=1)[CH3:22]

参加物

5

反応物 2

HCID 702EthanolHCID 23024912ethyl 3-(1-benzyl-3-ethoxy-1H-pyrazol-4-yl)propionate

生成物 1

HCID 178471163HCID 178471163、化合物収率 72%

試薬・触媒・溶媒 2

HCID 178418390HCID 178418390、化合物触媒HCID 284Formic Acid溶媒

実験手順

A mixture of ethyl 3-(1-benzyl-3-ethoxy-1H-pyrazol-4-yl)propionate (21.20 g), 5% palladium-carbon (40.00 g), ethanol (200 ml), and formic acid (100 ml) was refluxed for one hour. After the palladium-carbon was removed by filtration, the filtrate was concentrated. The residue was dissolved in ethyl acetate, which was washed with saturated aqueous sodium bicarbonate and then with saturated aqueous sodium chloride solution, dried (MgSO4), and then concentrated. The residue was subjected to silica gel column chromatography, and ethyl 3-(3-ethoxy-1H-pyrazol-4-yl)propionate (10.70 g, yield: 72%) was obtained as a colorless oily substance from the fraction eluted with ethyl acetate-hexane (1:1, volume ratio).

後処理

  1. temperaturewas refluxed for one hour
  2. customAfter the palladium-carbon was removed by filtration
  3. concentrationthe filtrate was concentrated
  4. dissolutionThe residue was dissolved in ethyl acetate
  5. washwhich was washed with saturated aqueous sodium bicarbonate
  6. dry with materialwith saturated aqueous sodium chloride solution, dried (MgSO4)
  7. concentrationconcentrated

出典と根拠

ORDレコード
ord-4a04574051114ad59289ac9bdfa1a414
出典データセット
uspto-grants-2007_02
特許番号
US07179823B1

反応ノート

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