Hydrochloric Acid → S 38093-2

HRID 1183801Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1183801
[CH2:1]1[C@H:5]2[CH2:6][CH2:7][CH2:8][C@H:4]2[CH2:3][N:2]1[CH2:9][CH2:10][CH2:11][O:12][C:13]1[CH:21]=[CH:20][C:16]([C:17]([NH2:19])=[O:18])=[CH:15][CH:14]=1.[ClH:22]>O>[ClH:22].[CH2:1]1[C@H:5]2[CH2:6][CH2:7][CH2:8][C@H:4]2[CH2:3][N:2]1[CH2:9][CH2:10][CH2:11][O:12][C:13]1[CH:14]=[CH:15][C:16]([C:17]([NH2:19])=[O:18])=[CH:20][CH:21]=1

Komponenten

4

Edukt 2

HCID 313Hydrochloric AcidHCID 709411121403835-45-9

Produkt 1

HCID 70945946S 38093-2Ausbeute 89 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel2×

Versuchsvorschrift

14.69 kg of 4-{3-[cis-hexahydrocyclopenta[c]pyrrol-2(1H)-yl]propoxy}benzamide and 122 L of water are introduced into a reactor. A solution of 6.81 kg of 37% hydrochloric acid in 11.54 L of water is also prepared. 13.75 kg of this acid solution are added to the reactor. The mixture is stirred for 1 hour at ambient temperature, and then for 1 hour 30 minutes at 60° C. The suspension is filtered in the hot state and the filter is then rinsed with water. A solvent change is then carried out on the filtrate, keeping the volume constant, in order to obtain an isopropanol/water ratio of 9/1. The product is isolated at 0° C. and the precipitate obtained is washed with isopropanol. The title product is finally obtained in a yield of 89% and with a chemical purity greater than 99%.

Aufarbeitung

  1. waitfor 1 hour 30 minutes at 60° C
  2. filtrationThe suspension is filtered in the hot state
  3. washthe filter is then rinsed with water
  4. customin order to obtain an isopropanol/water ratio of 9/1
  5. customThe product is isolated at 0° C.
  6. customthe precipitate obtained
  7. washis washed with isopropanol

Quellen und Nachweise

ORD-Eintrag
ord-d7eb3421550540a58a11bfd6c9621eb2
Quelldatensatz
uspto-grants-2014_03
Patentnummer
US08664408B2

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