Methanol → HCID 23690851、化合物

HRID 1456857ノート

反応式

HRID 1456857 の反応式
CO.[N:3]1[C:12]2[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=2)[CH:6]=[CH:5][C:4]=1[CH2:13][O:14][C:15]1[CH:20]=[CH:19][C:18]([C:21]([C:28]2[CH:33]=[CH:32][C:31]([O:34][CH2:35][C:36]3[CH:45]=[CH:44][C:43]4[C:38](=[CH:39][CH:40]=[CH:41][CH:42]=4)[N:37]=3)=[CH:30][CH:29]=2)([CH3:27])[CH2:22][CH2:23][C:24]([OH:26])=[O:25])=[CH:17][CH:16]=1.[OH-].[Na+:47]>O1CCOCC1>[Na+:47].[N:3]1[C:12]2[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=2)[CH:6]=[CH:5][C:4]=1[CH2:13][O:14][C:15]1[CH:20]=[CH:19][C:18]([C:21]([C:28]2[CH:33]=[CH:32][C:31]([O:34][CH2:35][C:36]3[CH:45]=[CH:44][C:43]4[C:38](=[CH:39][CH:40]=[CH:41][CH:42]=4)[N:37]=3)=[CH:30][CH:29]=2)([CH3:27])[CH2:22][CH2:23][C:24]([O-:26])=[O:25])=[CH:17][CH:16]=1

参加物

5

反応物 3

HCID 887MethanolHCID 14798Sodium HydroxideHCID 9850972HCID 9850972、化合物

生成物 1

HCID 23690851HCID 23690851、化合物

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

To a solution in dioxane (10 mL) and methanol (10 mL) of 4,4-bis(4-(2-quinolylmethoxy)phenyl)pentanoic acid (320 mg, 0.56 mmol), prepared as in step 1, was added aqueous 1N sodium hydroxide (0.55 ml, 0.55 mmol). The mixture was then concentrated in vacuo. The product was crystallized by dissolving in CH2Cl2 and precipitation by dropwise addition of a mixture of ethyl acetate-ethyl ether (1:2): 1 H NMR (300 MHz, DMSO-d6) d 1.47 (s, 3H), 1.63 (m, 2H), 2.18 (m, 2H), 5.31 (s, 4H), 6.95 (d, 4H, J=9 Hz), 7.08 (d, 4H, J=9 Hz), 7.64 (m, 4H), 7.78 (m, 2H), 8.00 (m, 4H), 8.40 (d, 2H, J=8 Hz); MS (FAB+) m/e 591 (M+H)+ ; (FAB-) 589 (M-H)-. Anal. Calc'd. for C37 H31N2O4Na.0.25 H2O:C, 74.67; H, 5.34; N, 4.71; Found: C, 74.57; H, 5.32; N, 4.52.

後処理

  1. concentrationThe mixture was then concentrated in vacuo
  2. customThe product was crystallized
  3. dissolutionby dissolving in CH2Cl2
  4. customprecipitation
  5. additionby dropwise addition of a mixture of ethyl acetate-ethyl ether (1:2)

出典と根拠

ORDレコード
ord-ae9ae6607d4947baa35de5b898e0b88d
出典データセット
uspto-grants-1998_12
特許番号
US05843968

反応ノート

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