Water → 1350343-61-1

HRID 919549Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 919549
Cl.[Cl:2][C:3]1[C:8]2[S:9][C:10]([C:12]([NH:14][C@@H:15]3[CH:20]4[CH2:21][CH2:22][N:17]([CH2:18][CH2:19]4)[CH2:16]3)=[O:13])=[CH:11][C:7]=2[CH:6]=[CH:5][CH:4]=1.O>C(#N)C>[OH2:13].[ClH:2].[Cl:2][C:3]1[C:8]2[S:9][C:10]([C:12]([NH:14][C@@H:15]3[CH:20]4[CH2:21][CH2:22][N:17]([CH2:18][CH2:19]4)[CH2:16]3)=[O:13])=[CH:11][C:7]=2[CH:6]=[CH:5][CH:4]=1

Komponenten

4

Edukt 2

HCID 962Water3×HCID 46208542Encenicline Hydrochloride2×

Produkt 1

HCID 545971881350343-61-1

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6342AcetonitrileLösungsmittel3×

Versuchsvorschrift

The present invention also provides another method for preparing the crystalline Form I, comprising: (a) heating 10-30% by weight of (R)-7-chloro-N-(quinuclidin-3-yl)benzo[b]thiophene-2-carboxamide hydrochloride in acetonitrile or an aqueous acetonitrile to between 60° C. and the boiling point of the solution, (b) optionally adding water to the mixture to fully dissolve the (R)-7-chloro-N-(quinuclidin-3-yl)benzo[b]thiophene-2-carboxamide hydrochloride; (c) cooling the solution until crystals are just visible; (d) if the water content is greater than 3% volume/volume when crystals are just visible, adding acetonitrile to the mixture so that the water content is less than 3% volume/volume; (e) cooling the resulting mixture to below 15° C.; and (f) isolating crystalline (R)-7-chloro-N-(quinuclidin-3-yl)benzo[b]thiophene-2-carboxamide hydrochloride monohydrate.

Aufarbeitung

  1. customThe present invention also provides another method
  2. customfor preparing the crystalline Form I

Quellen und Nachweise

ORD-Eintrag
ord-d1509c5d8c694cf9ad1879b94227988b
Quelldatensatz
uspto-grants-2016_03
Patentnummer
US09273044B2

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