Pyridine → HCID 178442765, Verbindung

HRID 1612600

Reaktionsgleichung

Reaktionsgleichung von HRID 1612600
[NH2:1][C:2]1[CH:7]=[C:6]([C:8]2[CH:13]=[CH:12][C:11]([CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH3:23])=[CH:10][CH:9]=2)[CH:5]=[CH:4][C:3]=1[OH:24].[CH2:25]([C@H:30]1[CH2:35][CH2:34][C@H:33]([C:36](Cl)=[O:37])[CH2:32][CH2:31]1)[CH2:26][CH2:27][CH2:28][CH3:29].O1CCOCC1.N1C=CC=CC=1>O>[CH2:25]([C@H:30]1[CH2:31][CH2:32][C@H:33]([C:36]([NH:1][C:2]2[CH:7]=[C:6]([C:8]3[CH:13]=[CH:12][C:11]([CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH3:23])=[CH:10][CH:9]=3)[CH:5]=[CH:4][C:3]=2[OH:24])=[O:37])[CH2:34][CH2:35]1)[CH2:26][CH2:27][CH2:28][CH3:29]

Komponenten

6

Edukt 4

HCID 1049PyridineHCID 312751,4-DioxaneHCID 197761232-Amino-4-(4-decylphenyl)phenolHCID 178444542HCID 178444542, Verbindung

Produkt 1

HCID 178442765HCID 178442765, VerbindungAusbeute 56,1 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

Step i) In a 50 ml-three-necked flask, 0.70 g (2.15 mM) of 2-amino-4-(4-decylphenyl)phenol, 0.48 g (2.21 mM) of trans-4-pentylcyclohexylcarbonyl chloride and 20 ml of dioxane were placed. To the mixture, 0.77 ml of pyridine was gradually added dropwise at about 87° C. under stirring, followed by heat-stirring for 1.5 hours at about 87° C. After the reaction, the reaction mixture was poured into 150 ml of water to precipitate a crystal. The crystal was recovered by filtration, washed with methanol and recrystallized from toluene to obtain 0.61 g of 2-(trans-4-pentylcyclohexylcarbonylamino)-4-(4-decylphenyl)phenol (yield: 56.1%).

Aufarbeitung

  1. stirringby heat-stirring for 1.5 hours at about 87° C
  2. customAfter the reaction
  3. customto precipitate a crystal
  4. filtrationThe crystal was recovered by filtration
  5. washwashed with methanol
  6. customrecrystallized from toluene

Quellen und Nachweise

ORD-Eintrag
ord-9aab12bd6b014cd887c05cf29b84ad58
Quelldatensatz
uspto-grants-1993_03
Patentnummer
US05190690

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