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4-Methyl-2-{5-[1-(4-methyl-pent-2-enyl)-piperidin-4-yl]-4'-trifluoromethyl-biphenyl-3-yl}-pentanoic acid ethyl ester → 4-Methyl-2-{5-[1-(4-methyl-pentyl)-piperidin-4-yl]-4'-trifluoromethyl-biphenyl-3-yl}-pentanoic acid ethyl ester

HRID 889761
ノート
印刷プレビュー

反応式

HRID 889761 の反応式
[CH2:1]([O:3][C:4](=[O:38])[CH:5]([C:10]1[CH:11]=[C:12]([C:28]2[CH:33]=[CH:32][C:31]([C:34]([F:37])([F:36])[F:35])=[CH:30][CH:29]=2)[CH:13]=[C:14]([CH:16]2[CH2:21][CH2:20][N:19]([CH2:22][CH:23]=[CH:24][CH:25]([CH3:27])[CH3:26])[CH2:18][CH2:17]2)[CH:15]=1)[CH2:6][CH:7]([CH3:9])[CH3:8])[CH3:2]>CO>[CH2:1]([O:3][C:4](=[O:38])[CH:5]([C:10]1[CH:11]=[C:12]([C:28]2[CH:29]=[CH:30][C:31]([C:34]([F:35])([F:36])[F:37])=[CH:32][CH:33]=2)[CH:13]=[C:14]([CH:16]2[CH2:17][CH2:18][N:19]([CH2:22][CH2:23][CH2:24][CH:25]([CH3:27])[CH3:26])[CH2:20][CH2:21]2)[CH:15]=1)[CH2:6][CH:7]([CH3:9])[CH3:8])[CH3:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

3

反応物 1

HCID 666982724-Methyl-2-{5-[1-(4-methyl-pent-2-enyl)-piperidin-4-yl]-4'-trifluoromethyl-biphenyl-3-yl}-pentanoic acid ethyl ester

生成物 1

HCID 576659734-Methyl-2-{5-[1-(4-methyl-pentyl)-piperidin-4-yl]-4'-trifluoromethyl-biphenyl-3-yl}-pentanoic acid ethyl ester

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A solution of a mixture of 4-methyl-2-{5-[1-(4-methyl-pent-2-enyl)-piperidin-4-yl]-4′-trifluoromethyl-biphenyl-3-yl}-pentanoic acid ethyl ester and methyl ester (69a) (25 mg, 0.05 mmol) in MeOH (2.0 mL) was flushed with N2. To this was added 10% Pd/C (5 mg). The suspension was hydrogenated at 20 psi for 4 h at room temperature. It was filtered through celite and the solid was washed with EtOAc. The filtrate was dried (MgSO4) and concentrated in vacuo to obtain 4-methyl-2-{5-[1-(4-methyl-pentyl)-piperidin-4-yl]-4′-trifluoromethyl-biphenyl-3-yl}-pentanoic acid ethyl ester and methyl ester. Calcd for C31H42F3NO2 (M+H) 518.67, Found 518.3 (methyl ester) and Calcd for C32H44F3NO2 (M+H) 532.69, Found 532.4 (ethyl ester).

後処理

  1. customwas flushed with N2
  2. additionTo this was added 10% Pd/C (5 mg)
  3. filtrationIt was filtered through celite
  4. washthe solid was washed with EtOAc
  5. dry with materialThe filtrate was dried (MgSO4)
  6. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-e0f8bd58c8364a7daac3a813c5fff830
出典データセット
uspto-grants-2012_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08252935B2

反応ノート

読み込み中…

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