Acetonitrile → 1350343-61-1

HRID 2370715Notes

Reaction equation

HRID 2370715 reaction equation
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.C(#N)C>O>[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

Participants

4

Reactant 2

HCID 6342Acetonitrile2×HCID 46208542Encenicline Hydrochloride2×

Product 1

HCID 545971881350343-61-1

Reagents, catalysts & solvents 1

HCID 962WaterSolvent2×

Procedure

The present invention further includes a method for preparing the crystalline Form II, the method comprising: (a) adding (R)-7-chloro-N-(quinuclidin-3-yl)benzo[b]thiophene-2-carboxamide hydrochloride to (i) acetonitrile or (ii) aqueous acetonitrile to create a composition that is 10-20% by weight of (R)-7-chloro-N-(quinuclidin-3-yl)benzo[b]thiophene-2-carboxamide hydrochloride; (b) optionally adding water to the composition to make the water content 6-10%; (c) optionally cooling the solution at below 10° C.; (d) allowing crystals to form; and (e) isolating crystalline (R)-7-chloro-N-(quinuclidin-3-yl)benzo[b]thiophene-2-carboxamide hydrochloride monohydrate.

Workup

  1. customto form

Sources & evidence

ORD record
ord-76481fee2efd40bba6cc47ee7296ec34
Source dataset
uspto-grants-2014_04
Patent number
US08710227B2

Reaction notes

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