4-[2-(Azetidin-1-yl)ethyl]piperazine-1-carboxylic acid [4-(4-nitrophenoxy)pyridin-2-yl]amide → 4-[2-(Azetidin-1-yl)ethyl]piperazine-1-carboxylic acid [4-(4-aminophenoxy)pyridin-2-yl]amide
反応式
[N+:1]([C:4]1[CH:31]=[CH:30][C:7]([O:8][C:9]2[CH:14]=[CH:13][N:12]=[C:11]([NH:15][C:16]([N:18]3[CH2:23][CH2:22][N:21]([CH2:24][CH2:25][N:26]4[CH2:29][CH2:28][CH2:27]4)[CH2:20][CH2:19]3)=[O:17])[CH:10]=2)=[CH:6][CH:5]=1)([O-])=O>O1CCCC1.CO.[C].[Pd]>[NH2:1][C:4]1[CH:5]=[CH:6][C:7]([O:8][C:9]2[CH:14]=[CH:13][N:12]=[C:11]([NH:15][C:16]([N:18]3[CH2:23][CH2:22][N:21]([CH2:24][CH2:25][N:26]4[CH2:29][CH2:28][CH2:27]4)[CH2:20][CH2:19]3)=[O:17])[CH:10]=2)=[CH:30][CH:31]=1参加物
5
反応物 1
生成物 1
試薬・触媒・溶媒 3
実験手順
4-[2-(Azetidin-1-yl)ethyl]piperazine-1-carboxylic acid [4-(4-nitrophenoxy)pyridin-2-yl]amide (122 mg) was dissolved in tetrahydrofuran (3 ml) and methanol (3 ml). 10% Palladium carbon (61 mg) was added, followed by stirring under a hydrogen atmosphere for 22 hrs. The reaction mixture was filtered to remove the catalyst, and the catalyst was washed with methanol. The filtrate was concentrated under reduced pressure to give a residue, which was then purified by silica gel column chromatography (Fuji Silysia NH, eluent; ethyl acetate:methanol=9:1). Fractions containing the target compound were concentrated to give a crude product of the titled compound (70 mg) as a pale yellow oil.
後処理
- filtrationThe reaction mixture was filtered
- customto remove the catalyst
- washthe catalyst was washed with methanol
- concentrationThe filtrate was concentrated under reduced pressure
- customto give a residue, which
- customwas then purified by silica gel column chromatography (Fuji Silysia NH, eluent; ethyl acetate:methanol=9:1)
- additionFractions containing the target compound
- concentrationwere concentrated
出典と根拠
- ORDレコード
- ord-9206415103584da38e5e506488c8a256
- 出典データセット
- uspto-grants-2009_05
- 特許番号
- US07531532B2
反応ノート
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