Acetic Acid → 4-Cyclohexylcyclohexylidenephosphorohydrazidic Acid, Diethyl Ester

HRID 1741927

Reaktionsgleichung

Reaktionsgleichung von HRID 1741927
[CH:1]1([CH:7]2[CH2:12][CH2:11][C:10](=O)[CH2:9][CH2:8]2)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.C(O)(=O)C.[P:18]([NH:26][NH2:27])(=[O:25])([O:22][CH2:23][CH3:24])[O:19][CH2:20][CH3:21]>C(Cl)Cl>[CH:1]1([CH:7]2[CH2:12][CH2:11][C:10](=[N:27][NH:26][P:18](=[O:25])([O:22][CH2:23][CH3:24])[O:19][CH2:20][CH3:21])[CH2:9][CH2:8]2)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1

Komponenten

5

Edukt 3

HCID 176Acetic AcidHCID 41690(1,1'-Bicyclohexyl)-4-oneHCID 143340Phosphorohydrazidic acid, diethyl ester

Produkt 1

HCID 855407454-Cyclohexylcyclohexylidenephosphorohydrazidic Acid, Diethyl Ester

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel2×

Versuchsvorschrift

To a solution of 4-cyclohexylcyclohexanone (27.04 g) and acetic acid (3 ml) in CH2Cl2 (400 ml) was added a solution of diethyl phosphorohydrazidate (28.91 g) in CH2Cl2 (100 ml). The reaction was stirred at room temperature for 27 hours and then was concentrated under reduced pressure. Toluene was added (2×) and removed under reduced pressure in order to aid in the removal of acetic acid by co-distillation. The residual yellow liquid was the product and was used without further purification. TLC Rf=0.52 (20% acetone in CH2Cl2, silica gel).

Aufarbeitung

  1. concentrationwas concentrated under reduced pressure
  2. additionToluene was added (2×)
  3. customremoved under reduced pressure in order
  4. customto aid in the removal of acetic acid by co-distillation
  5. customwas used without further purification

Quellen und Nachweise

ORD-Eintrag
ord-fd4344a22d3a443890f9862f1cefedc6
Quelldatensatz
uspto-grants-1994_08
Patentnummer
US05334712

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