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1-[2-(4-Bromophenoxy)ethyl]piperidine → 6-Methoxy-2-(4-Methoxyphenyl)-3-[4-[2-(1-Piperidinyl)ethoxy]phenyl]benzo[b]thiophene-3-Methanimine

HRID 850730
ノート
印刷プレビュー

反応式

HRID 850730 の反応式
[N:1]1([CH2:7][CH2:8][O:9][C:10]2[CH:15]=[CH:14][C:13](Br)=[CH:12][CH:11]=2)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.C([Li])(CC)C.[CH3:22][O:23][C:24]1[CH:25]=[CH:26][C:27]2[C:31]([C:32]#[N:33])=[C:30]([C:34]3[CH:39]=[CH:38][C:37]([O:40][CH3:41])=[CH:36][CH:35]=3)[S:29][C:28]=2[CH:42]=1>O1CCCC1>[CH3:22][O:23][C:24]1[CH:25]=[CH:26][C:27]2[C:31]([C:13]3[CH:14]=[CH:15][C:10]([O:9][CH2:8][CH2:7][N:1]4[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]4)=[CH:11][CH:12]=3)([CH:32]=[NH:33])[CH:30]([C:34]3[CH:35]=[CH:36][C:37]([O:40][CH3:41])=[CH:38][CH:39]=3)[S:29][C:28]=2[CH:42]=1
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 3

HCID 8671951-[2-(4-Bromophenoxy)ethyl]piperidineHCID 154582706-Methoxy-2-(4-methoxyphenyl)-1-benzothiophene-3-carbonitrileHCID 178418400CID 53628100

生成物 1

HCID 193650696-Methoxy-2-(4-Methoxyphenyl)-3-[4-[2-(1-Piperidinyl)ethoxy]phenyl]benzo[b]thiophene-3-Methanimine

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

To 4-[2-(1-piperidinyl)ethoxy]bromobenzene (114.5 mg, 0.357 mmol) in tetrahydrofuran (2 ml) at -78° C. is added secbutyl lithium (0.275 ml of a 1.3 M solution, 0.358 mmol). The resulting solution is stirred at that temperature for 30 minutes, then a solution of 6-methoxy-2-(4-methoxyphenyl)benzo[b]thiophene-3-carbonitrile (98.5 mg, 0.333 mmol) in tetrahydrofuran (1 ml) is added. The resulting mixture is stirred and allowed to warm to room temperature overnight. The reaction is then quenched by addition of saturated aqueous ammonium chloride (2 ml) and partitioned between methylene chloride and water. The layers are separated, and the aqueous layer extracted again with methylene chloride. The organic layers are combined, dried over magnesium sulfate, filtered and concentrated to an oil, which is chromatographed on silica gel (95:5:0.2 dichloromethane:methanol:triethylamine) to afford a fraction containing desired product. This fraction is concentrated and further chromatographed on silica gel (10:5:1 hexanes:dichloromethane:triethylamine) to afford, after drying in vacuo, 78.6 mg (47%) of title compound as an oil. IR (KBr) 2933, 1607, 1501, 1249, 1032 cm-1 ; 1H NMR (CDCl3): δ7.71 (d, 2 H, J=8.4 Hz), 7.42 (d, 2 H, J=8.7 Hz), 7.26 (m, 2 H), 6.90 (dd, 1 H, J=8.9, 2.2 Hz), 6.80 (m, 4 H), 4.10 (t, 2 H, J=6.0 Hz), 3.87 (s, 3 H), 3.76 (s, 3 H), 22.76 (t, 2 H, J=6.0 Hz), 2.50 (m, 4 H), 1.58 (m, 4 H), 1.44 (m, 2 H); 13C NMR (CDCl3): d 173.4, 161.4, 159.6, 157.7, 139.9, 138.5, 134.0, 131.1, 130.5, 129.9, 129.7, 125.9, 123.8, 114.7, 114.5, 114.2, 104.8, 66.2, 57.9, 55.7, 55.3, 55.1, 26.0, 24.3. Anal. Calcd. for C30H32N2O3S: C, 71.97; H, 6.44; N, 5.60; S, 6.40. Found: C, 71.73; H, 6.36; N, 5.41; S, 6.27.

後処理

  1. stirringThe resulting mixture is stirred
  2. customThe reaction is then quenched by addition of saturated aqueous ammonium chloride (2 ml)
  3. custompartitioned between methylene chloride and water
  4. customThe layers are separated
  5. extractionthe aqueous layer extracted again with methylene chloride
  6. dry with materialdried over magnesium sulfate
  7. filtrationfiltered
  8. concentrationconcentrated to an oil, which
  9. customis chromatographed on silica gel (95:5:0.2 dichloromethane:methanol:triethylamine)
  10. customto afford a fraction

出典と根拠

ORDレコード
ord-974401e24fb14ca6a43641b3f7d31821
出典データセット
uspto-grants-2000_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06018056

反応ノート

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