Water → Flecainide

HRID 1359121

Reaktionsgleichung

Reaktionsgleichung von HRID 1359121
C1(C)C=CC=CC=1.[NH2:8][CH2:9][CH:10]1[CH2:15][CH2:14][CH2:13][CH2:12][NH:11]1.O.[F:17][C:18]([F:42])([F:41])[CH2:19][O:20][C:21]1[CH:34]=[CH:33][C:32]([O:35][CH2:36][C:37]([F:40])([F:39])[F:38])=[CH:31][C:22]=1[C:23](OCC(F)(F)F)=[O:24]>CO>[CH:33]1[C:32]([O:35][CH2:36][C:37]([F:38])([F:39])[F:40])=[CH:31][C:22]([C:23]([NH:8][CH2:9][CH:10]2[NH:11][CH2:12][CH2:13][CH2:14][CH2:15]2)=[O:24])=[C:21]([O:20][CH2:19][C:18]([F:17])([F:41])[F:42])[CH:34]=1

Komponenten

6

Edukt 4

HCID 962WaterHCID 1140TolueneHCID 90865Piperidine-2-methylamineHCID 112810142,2,2-Trifluoroethyl 2,5-bis(2,2,2-trifluoroethoxy)benzoate

Produkt 1

HCID 3356Flecainide

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Reaktionsbedingungen

Temperatur
50 °C

Versuchsvorschrift

Dissolve in 48 ml of toluene 12.0 g (0.03 mol) of trifluoroethanol 2,5-bis-trifluoroethoxybenzoate. Add 3.94 g (0.0345 mol) of 2-aminomethylpiperidine and heat the solution to a temperature of 80°±5° C. for 8 hours. Cool to 50° C. and add 36 ml of water. Carry out the separation at a temperature of 45°±5° C. Concentrate the organic phase under vacuum at a temperature of 35°±5° C. so as to eliminate as much toluene as possible. A semi-solid residue is obtained which is dissolved in 20 ml of methanol and concentrated again to a residue under vacuum. Methanol (40 ml) is then added and heated with refluxing until a yellow solution is obtained. Then cool until the crude base crystallizes, the precipitation is completed by adding 40 ml of water.

Aufarbeitung

  1. temperatureheat the solution to a temperature of 80°±5° C. for 8 hours
  2. customCarry out the separation at a temperature of 45°±5° C
  3. concentrationConcentrate the organic phase under vacuum at a temperature of 35°±5° C. so as
  4. customA semi-solid residue is obtained which
  5. concentrationconcentrated again to a residue under vacuum
  6. additionMethanol (40 ml) is then added
  7. temperatureheated
  8. temperaturewith refluxing until a yellow solution
  9. customis obtained
  10. customcrystallizes
  11. customthe precipitation
  12. additionby adding 40 ml of water

Quellen und Nachweise

ORD-Eintrag
ord-fd062efa44324b67b5831a945dd1e406
Quelldatensatz
uspto-grants-2003_07
Patentnummer
US06599922B2

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