HCID 86229373、化合物 → 1-((6-ethylpyridin-3-yl)methyl)-5-(4-methoxyphenyl)pyridin-2(1H)-one

HRID 1948281ノート

反応式

HRID 1948281 の反応式
[C:1]([C:3]1[N:8]=[CH:7][C:6]([CH2:9][N:10]2[CH:15]=[C:14]([C:16]3[CH:21]=[CH:20][C:19]([O:22][CH3:23])=[CH:18][CH:17]=3)[CH:13]=[CH:12][C:11]2=[O:24])=[CH:5][CH:4]=1)#[CH:2]>CO.[Pd]>[CH2:1]([C:3]1[N:8]=[CH:7][C:6]([CH2:9][N:10]2[CH:15]=[C:14]([C:16]3[CH:17]=[CH:18][C:19]([O:22][CH3:23])=[CH:20][CH:21]=3)[CH:13]=[CH:12][C:11]2=[O:24])=[CH:5][CH:4]=1)[CH3:2]

参加物

4

反応物 1

HCID 86229373HCID 86229373、化合物

生成物 1

HCID 589669071-((6-ethylpyridin-3-yl)methyl)-5-(4-methoxyphenyl)pyridin-2(1H)-one収率 62.4%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 887Methanol溶媒

実験手順

According to Scheme 33 Step 3: To a suspension of Pd/C 10% (0.05 eq) in MeOH (10 mL) under N2 atmosphere, a solution of 1-((6-ethynylpyridin-3-yl)methyl)-5-(4-methoxyphenyl)pyridin-2(1H)-one (0.15 mmol, 48 mg) was added at room temperature. The flask was evacuated and filled with hydrogen until the pressure reached 20 psi. The resulting suspension was shaken at room temperature for 1 hour. The catalyst was filtered off and the filtrate was evaporated under vacuum to give a residue. The residue was purified in a circular chromatography-TLC CH2Cl2/MeOH(NH3)sat. 2% yielding 1-((6-ethylpyridin-3-yl)methyl)-5-(4-methoxyphenyl)pyridin-2(1H)-one (30 mg, 61%).

後処理

  1. customThe flask was evacuated
  2. additionfilled with hydrogen until the pressure
  3. filtrationThe catalyst was filtered off
  4. customthe filtrate was evaporated under vacuum
  5. customto give a residue
  6. customThe residue was purified in a circular chromatography-TLC CH2Cl2/MeOH(NH3)sat

出典と根拠

ORDレコード
ord-9dc32c85029c47c7a30744927bdcf862
出典データセット
uspto-grants-2013_03
特許番号
US08399493B2

反応ノート

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