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Ethanol → ethyl 1-acetyl-2,3-dihydro-5-methoxy-1H-indole-2-carboximidate monohydrochloride

HRID 887925
Notes
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Reaction equation

HRID 887925 reaction equation
[C:1]([N:4]1[C:12]2[C:7](=[CH:8][C:9]([O:13][CH3:14])=[CH:10][CH:11]=2)[CH2:6][CH:5]1[C:15]#[N:16])(=[O:3])[CH3:2].[CH2:17]([OH:19])[CH3:18].[ClH:20].C(OCC)C>>[ClH:20].[C:1]([N:4]1[C:12]2[C:7](=[CH:8][C:9]([O:13][CH3:14])=[CH:10][CH:11]=2)[CH2:6][CH:5]1[C:15](=[NH:16])[O:19][CH2:17][CH3:18])(=[O:3])[CH3:2]
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

4

Reactant 3

HCID 702EthanolHCID 10953452Ether hydrochlorideHCID 219141141-acetyl-2,3-dihydro-5-methoxy-1H-indole-2-carbonitrile

Product 1

HCID 21914094ethyl 1-acetyl-2,3-dihydro-5-methoxy-1H-indole-2-carboximidate monohydrochloride

Procedure

To a solution of intermediate (23) (0.0154 mole) and ethanol (0.0231 mole) in 1M HCl/diethylether (200 ml), cooled in an ice bath was bubbled HCl (gas) for 60 minutes. The ice bath was maintained for 45 minutes, and the mixture was concentrated at room temperature under vacuum to 200 ml of an oily precipitate. The residue was triturated to a brown solid that became an oil after decanting off the diethylether. The residue was washed with diethylether twice, dissolved in methanol, and used without further purification for further synthesis, yielding ethyl 1-acetyl-2,3-dihydro-5-methoxy-1H-indole-2-carboximidate monohydrochloride (intermediate 24).

Workup

  1. customwas bubbled HCl (gas) for 60 minutes
  2. temperatureThe ice bath was maintained for 45 minutes
  3. concentrationthe mixture was concentrated at room temperature under vacuum to 200 ml of an oily precipitate
  4. customThe residue was triturated to a brown solid that
  5. customafter decanting off the diethylether
  6. washThe residue was washed with diethylether twice
  7. dissolutiondissolved in methanol
  8. customused without further purification for further synthesis

Sources & evidence

ORD record
ord-630b172f0b51487eb3e9de8ff6ea89d5
Source dataset
uspto-grants-2012_08
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US08247432B2

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes