Hydrochloric Acid → HCID 10429825, compound

HRID 1489151Notes

Reaction equation

HRID 1489151 reaction equation
[C:1]1([CH:7]2[C:15]3[C:10](=[CH:11][CH:12]=[CH:13][CH:14]=3)[N:9]([C:16]([CH:18]3[CH2:26][CH2:25][C:21]4[N:22]=[CH:23][NH:24][C:20]=4[CH2:19]3)=[O:17])[CH2:8]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[ClH:27]>C(O)C.C(OCC)(=O)C>[ClH:27].[C:1]1([CH:7]2[C:15]3[C:10](=[CH:11][CH:12]=[CH:13][CH:14]=3)[N:9]([C:16]([CH:18]3[CH2:26][CH2:25][C:21]4[N:22]=[CH:23][NH:24][C:20]=4[CH2:19]3)=[O:17])[CH2:8]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

Participants

5

Reactant 2

HCID 313Hydrochloric AcidHCID 98410295-(3-Phenylindolin-1-ylcarbonyl)-4,5,6,7-tetrahydrobenzimidazole

Product 1

HCID 10429825HCID 10429825, compound

Reagents, catalysts & solvents 2

HCID 702EthanolSolventHCID 8857Ethyl AcetateSolvent2×

Procedure

A 100 mg portion of the 5-[(3-phenylindolin-1-yl)carbonyl]-4,5,6,7-tetrahydrobenzimidazole produced in the preferred embodiment 1 was dissolved in 3 ml ethanol, and 0.4 ml of 4N hydrogen chloride solution in ethyl acetate was added under ice cooling. The solution was concentrated under reduced pressure to obtain a partially oily residue. After adding 5 ml of ethyl acetate thereto and stirring, the insoluble portion was collected by filtration to obtain the 5-[(3-phenylindolin-1-yl)carbonyl]-4,5,6,7-tetrahydrobenziamidazole hydrochloride (compound 2) listed in the above heading.

Workup

  1. concentrationThe solution was concentrated under reduced pressure
  2. customto obtain a partially oily residue
  3. filtrationthe insoluble portion was collected by filtration

Sources & evidence

ORD record
ord-a01ffa1ff91940aeb4482a60e1ebf4c7
Source dataset
uspto-grants-1997_10
Patent number
US05677326

Reaction notes

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