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N-[(3R)-1-azabicyclo[2.2.2]oct-3-yl]-3-chloro-6-nitro-1-benzothiophene-2-carboxamide hydrochloride → N-[(3R)-1-Azabicyclo[2.2.2]oct-3-yl]-3-chloro-6-amino-1-benzothiophene-2-carboxamide dihydrochloride

HRID 335610
Notes
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Reaction equation

HRID 335610 reaction equation
[ClH:1].[N:2]12[CH2:9][CH2:8][CH:5]([CH2:6][CH2:7]1)[C@@H:4]([NH:10][C:11]([C:13]1[S:14][C:15]3[CH:22]=[C:21]([N+:23]([O-])=O)[CH:20]=[CH:19][C:16]=3[C:17]=1[Cl:18])=[O:12])[CH2:3]2>[Sn](Cl)Cl.CN(C=O)C>[ClH:18].[ClH:1].[N:2]12[CH2:7][CH2:6][CH:5]([CH2:8][CH2:9]1)[C@@H:4]([NH:10][C:11]([C:13]1[S:14][C:15]3[CH:22]=[C:21]([NH2:23])[CH:20]=[CH:19][C:16]=3[C:17]=1[Cl:18])=[O:12])[CH2:3]2
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

4

Reactant 1

HCID 68431015N-[(3R)-1-azabicyclo[2.2.2]oct-3-yl]-3-chloro-6-nitro-1-benzothiophene-2-carboxamide hydrochloride

Product 1

HCID 68431670N-[(3R)-1-Azabicyclo[2.2.2]oct-3-yl]-3-chloro-6-amino-1-benzothiophene-2-carboxamide dihydrochloride

Reagents, catalysts & solvents 2

HCID 6228DimethylformamideSolventHCID 24479Stannous ChlorideSolvent

Procedure

83 mg (0.23 mmol) of N-[(3R)-1-azabicyclo[2.2.2]oct-3-yl]-3-chloro-6-nitro-1-benzothiophene-2-carboxamide hydrochloride are dissolved in 1.5 ml of 2M tin(II) chloride solution in DMF and stirred at RT for 14 h. The reaction mixture is purified by preparative HPLC. The product fractions are concentrated, dissolved in a mixture of methanol and 4M HCl in dioxane, then again concentrated and dried under high vacuum. 53 mg (57.2% of theory) of the title compound are obtained.

Workup

  1. customThe reaction mixture is purified by preparative HPLC
  2. concentrationThe product fractions are concentrated
  3. dissolutiondissolved in a mixture of methanol and 4M HCl in dioxane
  4. concentrationagain concentrated
  5. customdried under high vacuum

Sources & evidence

ORD record
ord-b299223a520a442ab1cb517011e77954
Source dataset
uspto-grants-2014_11
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US08884017B2

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes