4-Nitrophenol → HCID 68746508, Verbindung

HRID 1886885

Reaktionsgleichung

Reaktionsgleichung von HRID 1886885
[C:1]([OH:26])(=[O:25])[CH2:2][CH2:3][C@H:4]([C@@H:6]1[C@:23]2([CH3:24])[C@H:9]([C@H:10]3[C@H:20]([CH2:21][CH2:22]2)[C@:18]2([CH3:19])[CH:13]([CH2:14][CH2:15][CH2:16][CH2:17]2)[CH2:12][CH2:11]3)[CH2:8][CH2:7]1)[CH3:5].[N+:27]([C:30]1[CH:35]=[CH:34][C:33](O)=[CH:32][CH:31]=1)([O-:29])=[O:28].C1(N=C=NC2CCCCC2)CCCCC1>C(Cl)Cl.C(OCC)(=O)C>[N+:27]([C:30]1[CH:35]=[CH:34][C:33]([O:25][C:1](=[O:26])[CH2:2][CH2:3][C@H:4]([C@@H:6]2[C@:23]3([CH3:24])[C@H:9]([C@H:10]4[C@H:20]([CH2:21][CH2:22]3)[C@:18]3([CH3:19])[CH:13]([CH2:14][CH2:15][CH2:16][CH2:17]3)[CH2:12][CH2:11]4)[CH2:8][CH2:7]2)[CH3:5])=[CH:32][CH:31]=1)([O-:29])=[O:28]

Komponenten

6

Edukt 3

HCID 9804-NitrophenolHCID 10868DicyclohexylcarbodiimideHCID 9548797Cholanic acid

Produkt 1

HCID 68746508HCID 68746508, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 6344DichloromethaneLösungsmittelHCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

Cholanic acid (3.6 g, 10.0 mmoles) is suspended in methylene chloride (200 mL) and stirred well at ambient temperature. 4-Nitrophenol (1.4 g, 10.1 mmoles) and N,N′-dicylcohexylcarbodiimide (2.1 g, 10.2 mmoles) are added, and the mixture is stirred overnight. The mixture is then filtered, the solid washed with a little methylene chloride, and the filtrate is evaporated to dryness to give a yellow solid. The crude product is dissolved in ethyl acetate (100 mL). The solution is filtered and the filtrate si evaporated to give an off-white solid. The solid is crystallized from hot hexanes. The yield is 3.9 g (80%).

Aufarbeitung

  1. stirringthe mixture is stirred overnight
  2. filtrationThe mixture is then filtered
  3. washthe solid washed with a little methylene chloride
  4. customthe filtrate is evaporated to dryness
  5. customto give a yellow solid
  6. filtrationThe solution is filtered
  7. customthe filtrate si evaporated
  8. customto give an off-white solid
  9. customThe solid is crystallized from hot hexanes

Quellen und Nachweise

ORD-Eintrag
ord-c62d157395b9420c92528e0fe5fdd6e5
Quelldatensatz
uspto-grants-2013_08
Patentnummer
US08501706B2

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