Potassium Hydroxide → HCID 11276773、化合物

HRID 1059695ノート

反応式

HRID 1059695 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[CH2:9][CH2:10][N:11]([CH2:14][CH2:15][CH2:16][NH:17]C(=O)C(F)(F)F)[CH2:12][CH:13]=2)=[CH:4][CH:3]=1.[OH-].[K+]>C(O)C>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[CH2:13][CH2:12][N:11]([CH2:14][CH2:15][CH2:16][NH2:17])[CH2:10][CH:9]=2)=[CH:4][CH:3]=1

参加物

4

反応物 2

HCID 14797Potassium HydroxideHCID 18630938HCID 18630938、化合物

生成物 1

HCID 11276773HCID 11276773、化合物収率 64.1%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

N-{3-[4-(4-Chloro-phenyl)-3,6-dihydro-2H-pyridin-1-yl]-propyl}-2,2,2-trifluoroacetamide (1.77 g, 5.10 mmol) and 20% aqueous KOH (25 mL) in ethanol (50 mL) were stirred at room temperature for 30 minutes. The reaction mixture was concentrated to dryness and the solids were washed with methylene chloride, dried over magnesium sulfate and concentrated to give 3-[4-(4-Chloro-phenyl)-3,6-dihydro-2H-pyridin-1-yl]-propylamine (0.82 g, 64%) as a waxy white solid. Mp. 57-58° C.; NMR CDCl3 δ 7.29-7.20 (m, 4H), 6.03 (s, 1H), 3.12 (d, J=3.3 Hz, 2H), 2.76 (t, J=6.9 Hz, 2H), 2.67 (t, J=5.6 Hz, 2H), 2.51-2.44 (m, 4H), 1.69 (p, J=7.5 Hz, 2H), 1.63 (s, 2H); 13C NMR CDCl3 δ 139.20, 133.96, 132.61, 128.36, 126.15, 122.41, 56.20, 53.36, 50.30, 40.77, 30.73, 28.01; IR(KBr) 2929, 2861, 2805, 2767, 2734, 1493, 1467, 1379, 1320, 1128, 1095, 845, 825, 800; Analysis calculated for C14H19CIN2.0.25H2O: C, 65.87; H, 7.70; N, 10.97. Found: C, 65.69; H, 7.44; N, 10.91.

後処理

  1. concentrationThe reaction mixture was concentrated to dryness
  2. washthe solids were washed with methylene chloride
  3. dry with materialdried over magnesium sulfate
  4. concentrationconcentrated

出典と根拠

ORDレコード
ord-4d1c9290411140e094453b77383fb627
出典データセット
uspto-grants-2003_02
特許番号
US06521630B1

反応ノート

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