HCID 489113、化合物 → HCID 510558、化合物

HRID 843166ノート

反応式

HRID 843166 の反応式
[CH2:1]([O:3][C:4]([C:6]1[O:7][C:8]2[CH:15]=[CH:14][CH:13]=[C:12]([O:16][CH2:17][CH2:18][CH2:19][NH:20]CC3C=CC=CC=3)[C:9]=2[C:10]=1[CH3:11])=[O:5])[CH3:2].[H][H]>C1COCC1.[OH-].[OH-].[Pd+2]>[CH2:1]([O:3][C:4]([C:6]1[O:7][C:8]2[CH:15]=[CH:14][CH:13]=[C:12]([O:16][CH2:17][CH2:18][CH2:19][NH2:20])[C:9]=2[C:10]=1[CH3:11])=[O:5])[CH3:2]

参加物

5

反応物 2

HCID 489113HCID 489113、化合物HCID 178418361HCID 178418361、化合物

生成物 1

HCID 510558HCID 510558、化合物

試薬・触媒・溶媒 2

HCID 9942167Palladium hydroxide触媒HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution of 4-(3-benzylamino-propoxy)-3-methyl-benzofuran-2-carboxylic acid ethyl ester (the compound in Example 98: 180 mg) in THF (10 ml) was added 20% Pd(OH)2 on charcoal catalyst (40 mg) under N2. The nitrogen atmosphere was replaced by hydrogen (1 atom) and the resulting mixture was stirred overnight at room temperature. The reaction mixture was filtered through a pad of celite and the pad of celite was rinsed with methanol and dichloromethane. The filtrate combined was concentrated in vacuo. The residue was purified by silica gel column chromatography (dichloromethane-MeOH) to give 4-(3-amino-propoxy)-3-methyl-benzofuran-2-carboxylic acid ethyl ester (125 mg) as a colorless oil. FAB-MS: m/z 278 (MH+).

後処理

  1. filtrationThe reaction mixture was filtered through a pad of celite
  2. washthe pad of celite was rinsed with methanol and dichloromethane
  3. concentrationThe filtrate combined was concentrated in vacuo
  4. customThe residue was purified by silica gel column chromatography (dichloromethane-MeOH)

出典と根拠

ORDレコード
ord-a9d9bce8dfb24c2fb4ddf83dacb5fed9
出典データセット
uspto-grants-2002_04
特許番号
US06376491B1

反応ノート

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