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Methanol → Methyl 1-amino-4-methoxy-4-(trifluoromethyl)cyclohexanecarboxylate

HRID 922126
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 922126
[NH2:1][C:2]1([C:14]([OH:16])=[O:15])[CH2:7][CH2:6][C:5]([O:12][CH3:13])([C:8]([F:11])([F:10])[F:9])[CH2:4][CH2:3]1.S(Cl)(Cl)=O.[CH3:21]O>>[NH2:1][C:2]1([C:14]([O:16][CH3:21])=[O:15])[CH2:7][CH2:6][C:5]([O:12][CH3:13])([C:8]([F:11])([F:10])[F:9])[CH2:4][CH2:3]1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 3

HCID 887MethanolHCID 24386Thionyl Chloride3×HCID 904137291-Amino-4-methoxy-4-(trifluoromethyl)cyclohexanecarboxylic acid

Produkt 1

HCID 71246475Methyl 1-amino-4-methoxy-4-(trifluoromethyl)cyclohexanecarboxylate

Versuchsvorschrift

12.20 g (corresponds to about 37.58 mmol) of 1-amino-4-methoxy-4-(trifluoromethyl)cyclohexanecarboxylic acid (Example 18A) were suspended in 210 ml of methanol, and 10.4 ml (142.80 mmol) of thionyl chloride were added at 0° C. The mixture was boiled under reflux for 2 hours and cooled, another 10.4 ml (142.80 mmol) of thionyl chloride were added at 0° C. and the mixture was boiled under reflux for a further 2 hours. The reaction was cooled, another 10.4 ml (142.80 mmol) of thionyl chloride were added and the mixture was heated at reflux overnight until the reaction had gone to completion. For work-up, about 100 ml of methanol were distilled off and the concentrate was poured into 1 l of saturated aqueous sodium carbonate solution. The product was extracted with ethyl acetate and the organic phase was dried over sodium sulphate. Concentration by evaporation gave 7.01 g (73% of theory) of the title compound as a yellowish oil.

Aufarbeitung

  1. temperatureunder reflux for 2 hours
  2. temperaturecooled
  3. temperatureunder reflux for a further 2 hours
  4. temperatureThe reaction was cooled
  5. temperaturethe mixture was heated
  6. temperatureat reflux overnight until the reaction
  7. distillationFor work-up, about 100 ml of methanol were distilled off
  8. additionthe concentrate was poured into 1 l of saturated aqueous sodium carbonate solution
  9. extractionThe product was extracted with ethyl acetate
  10. dry with materialthe organic phase was dried over sodium sulphate
  11. concentrationConcentration
  12. customby evaporation

Quellen und Nachweise

ORD-Eintrag
ord-d4e0852c25294342b9351ba61810761f
Quelldatensatz
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US09278925B2

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