HCID 67429355、化合物 → HCID 86625703、化合物

HRID 1662669ノート

反応式

HRID 1662669 の反応式
C(OC(=O)[N:10]([CH2:18][CH2:19][O:20]CC1C=CC=CC=1)[C@@H:11]([CH3:17])[C:12]([N:14]([CH3:16])[CH3:15])=[O:13])C1C=CC=CC=1.[H][H]>CCO.[Pd]>[OH:20][CH2:19][CH2:18][NH:10][C@@H:11]([CH3:17])[C:12]([N:14]([CH3:16])[CH3:15])=[O:13]

参加物

5

反応物 2

HCID 67429355HCID 67429355、化合物HCID 178418361HCID 178418361、化合物

生成物 1

HCID 86625703HCID 86625703、化合物収率 64.1%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 702Ethanol溶媒

反応条件

温度
45 °C

実験手順

Under nitrogen atmosphere, to a solution of 2.75 g of the compound obtained in Step 79-2 in EtOH (30 ml) was added palladium-activated carbon (10% Pd, 0.30 g), and the inside of the reaction system was displaced with hydrogen gas. The solution was stirred for 24 hours at 45° C., then, the reaction solution was filtered, and the solvent was filtered out under reduced pressure. To a solution of the obtained residue in EtOH (30 ml) solution was added palladium-activated carbon (10% Pd, 0.30 g), and the reaction system was displaced with hydrogen gas, again. The solution was stirred for one day at 45° C., then, the reaction solution was filtered, and the solvent was evaporated under reduced pressure. The obtained residue was purified by column chromatography (silicagel 60; mobile phase: CHCl3/MeOH=9/1 to 4/1; v/v) to obtain 734 mg of the title compound (colorless oil).

後処理

  1. filtrationthe reaction solution was filtered
  2. filtrationthe solvent was filtered out under reduced pressure
  3. additionTo a solution of the obtained residue in EtOH (30 ml) solution was added palladium-activated carbon (10% Pd, 0.30 g)
  4. stirringThe solution was stirred for one day at 45° C.
  5. filtrationthe reaction solution was filtered
  6. customthe solvent was evaporated under reduced pressure
  7. customThe obtained residue was purified by column chromatography (silicagel 60; mobile phase: CHCl3/MeOH=9/1 to 4/1; v/v)

出典と根拠

ORDレコード
ord-36421ef84bcf4397a2eca8bf46779876
出典データセット
uspto-grants-2011_10
特許番号
US08030499B2

反応ノート

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