1-Benzyl-4-(2-methyl-4-pyridinyl)piperazine → 1-(2-Methylpyridin-4-yl)piperazine
反応式
C([N:8]1[CH2:13][CH2:12][N:11]([C:14]2[CH:19]=[CH:18][N:17]=[C:16]([CH3:20])[CH:15]=2)[CH2:10][CH2:9]1)C1C=CC=CC=1>[C].[Pd].CO>[CH3:20][C:16]1[CH:15]=[C:14]([N:11]2[CH2:12][CH2:13][NH:8][CH2:9][CH2:10]2)[CH:19]=[CH:18][N:17]=1参加物
4
実験手順
1-Benzyl-4-(2-methyl-4-pyridinyl)piperazine (10.3 g) obtained in Example 114a) and 10% palladium carbon (1.0 g) were added to methanol (200 ml), and mixed under hydrogen atmosphere at room temperature for 7 days. The catalyst was filtered off, and the filtrate was concentrated under reduced pressure. The residue was purified with basic silica gel column (ethyl acetate) and recrystallized from ethyl acetate-hexane to obtain the title compound as a colorless needle-like crystal (2.58 g, 38%).
後処理
- additionmixed under hydrogen atmosphere at room temperature for 7 days
- filtrationThe catalyst was filtered off
- concentrationthe filtrate was concentrated under reduced pressure
- customThe residue was purified with basic silica gel column (ethyl acetate)
- customrecrystallized from ethyl acetate-hexane
出典と根拠
- ORDレコード
- ord-ebdfc00d2e2241ed8e23c40344042e29
- 出典データセット
- uspto-grants-2010_10
- 特許番号
- US07820673B2
反応ノート
読み込み中…