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1-[2-Methyl-5-(methyloxy)-4-nitrophenyl]-4-[2-(methylsulfonyl)ethyl]piperidine → 5-Methyl-2-(methyloxy)-4-{4-[2-(methylsulfonyl)ethyl]-1-piperidinyl}aniline

HRID 419620
ノート
印刷プレビュー

反応式

HRID 419620 の反応式
[CH3:1][C:2]1[CH:7]=[C:6]([N+:8]([O-])=O)[C:5]([O:11][CH3:12])=[CH:4][C:3]=1[N:13]1[CH2:18][CH2:17][CH:16]([CH2:19][CH2:20][S:21]([CH3:24])(=[O:23])=[O:22])[CH2:15][CH2:14]1>CCOC(C)=O.CO.[Pt]>[CH3:1][C:2]1[C:3]([N:13]2[CH2:18][CH2:17][CH:16]([CH2:19][CH2:20][S:21]([CH3:24])(=[O:22])=[O:23])[CH2:15][CH2:14]2)=[CH:4][C:5]([O:11][CH3:12])=[C:6]([CH:7]=1)[NH2:8]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 1

HCID 594526541-[2-Methyl-5-(methyloxy)-4-nitrophenyl]-4-[2-(methylsulfonyl)ethyl]piperidine

生成物 1

HCID 594526535-Methyl-2-(methyloxy)-4-{4-[2-(methylsulfonyl)ethyl]-1-piperidinyl}aniline収率 83.6%

試薬・触媒・溶媒 3

HCID 23939Platinum触媒HCID 887Methanol溶媒HCID 8857Ethyl Acetate溶媒2 回

実験手順

To 1-[2-methyl-5-(methyloxy)-4-nitrophenyl]-4-[2-(methylsulfonyl)ethyl]piperidine (26 g, 73 mmol) in EtOAc (1 L) and MeOH (200 mL) was added platinum on carbon (sulfided) (14 g, 73 mmol) as a slurry in EtOAc (100 mL). The mixture was stirred under H2 (1 atm.) for 2 days. The catalyst was filtered off and rinsed with EtOAc, MeOH, and DCM and the filtrate was rotovapped down. The resultant solid was triturated with diethyl ether to provide the title compound of Step J (20 g, 61 mmol, 82%). 1H NMR (400 MHz, DMSO-d6) δ 6.50 (s, 1H), 6.39 (s, 1H), 4.24 (s, 2H), 3.66 (s, 3H), 3.05-3.16 (m, 2H), 2.92 (s, 3H), 2.83 (d, 2H), 2.39-2.54 (m, 2H), 2.01 (s, 3H), 1.55-1.76 (m, 4H), 1.32-1.46 (m, J=10.6, 7.0, 3.5, 3.5 Hz, 1H), 1.24 (qd, J=11.7, 3.4 Hz, 2H).

後処理

  1. filtrationThe catalyst was filtered off
  2. washrinsed with EtOAc, MeOH, and DCM
  3. customThe resultant solid was triturated with diethyl ether

出典と根拠

ORDレコード
ord-2ccbf6c6501c4bafbee435c19c3af6e4
出典データセット
uspto-grants-2012_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08093239B2

反応ノート

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