4-Methylmorpholine → 1,4-Cyclohexanedimethanol

HRID 1017108

Reaktionsgleichung

Reaktionsgleichung von HRID 1017108
[C@H:1]1([CH2:9][OH:10])[CH2:6][CH2:5][C@H:4]([CH2:7][OH:8])[CH2:3][CH2:2]1.CN1CCOCC1.P(Cl)(Cl)(=O)OCCCCCC>C(Cl)Cl>[CH2:3]1[CH:4]([CH2:7][OH:8])[CH2:5][CH2:6][CH:1]([CH2:9][OH:10])[CH2:2]1

Komponenten

5

Edukt 3

HCID 79724-MethylmorpholineHCID 6422909Phosphorodichloridic acid, hexyl esterHCID 178520956HCID 178520956, Verbindung

Produkt 1

HCID 77351,4-Cyclohexanedimethanol

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel3×

Reaktionsbedingungen

Temperatur
-40 °C

Versuchsvorschrift

Under an argon stream, 10 g of trans-1,4-cyclohexane dimethanol (CHDM), 15.25 mL (14.03 g) of N-methyl morpholine (NMM), and 50 mL of methylene chloride were transferred into a 250 mL flash equipped with a funnel. The solution in the flask was cooled down to −40° C. with stirring. A solution of 15.19 g of hexyl phosphoro-dichloridate (HOP) in 20 mL of methylene chloride was added through the funnel, and an additional 10 mL of methylene chloride was used to flush through the funnel. The mixture was then brought up to room temperature gradually and kept stirring for four hours.

Aufarbeitung

  1. customequipped with a funnel
  2. customto flush through the funnel
  3. customwas then brought up to room temperature
  4. stirringkept stirring for four hours

Quellen und Nachweise

ORD-Eintrag
ord-df1d02226a804957acf2793c9287c89a
Quelldatensatz
uspto-grants-2002_11
Patentnummer
US06479067B2

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