Hydrogen chloride-ethyl acetate → HCID 67538582, compound

HRID 39786Notes

Reaction equation

HRID 39786 reaction equation
[O:1]1[C:6]2[CH:7]=[CH:8][C:9]([CH2:11][NH:12][CH:13]3[CH2:18][CH2:17][N:16]([CH2:19][CH2:20][N:21]4[C:30]5[C:25](=[CH:26][CH:27]=[CH:28][CH:29]=5)[N:24]=[CH:23][C:22]4=[O:31])[CH2:15][CH2:14]3)=[CH:10][C:5]=2[O:4][CH2:3][CH2:2]1.[ClH:32].C(OCC)(=O)C>C(OCC)(=O)C>[ClH:32].[O:1]1[C:6]2[CH:7]=[CH:8][C:9]([CH2:11][NH:12][CH:13]3[CH2:18][CH2:17][N:16]([CH2:19][CH2:20][N:21]4[C:30]5[C:25](=[CH:26][CH:27]=[CH:28][CH:29]=5)[N:24]=[CH:23][C:22]4=[O:31])[CH2:15][CH2:14]3)=[CH:10][C:5]=2[O:4][CH2:3][CH2:2]1

Participants

4

Reactant 2

HCID 21866389Hydrogen chloride-ethyl acetateHCID 59398270HCID 59398270, compound

Product 1

HCID 67538582HCID 67538582, compound

Reagents, catalysts & solvents 1

HCID 8857Ethyl AcetateSolvent2×

Procedure

To 5 mL of an ethyl acetate solution containing 0.15 g of 1-(2-(4-((2,3-dihydro-1,4-benzodioxin-6-ylmethyl)amino)piperidin-1-yl)ethyl)quinoxalin-2(1H)-one, 5 mL of 4.0 mol/L hydrogen chloride/ethyl acetate was added at room temperature. The mixture was stirred at the same temperature for 10 min, and the solvent was removed under reduced pressure. To the residue thus obtained, ethyl acetate was added and the resulting solid was filtered to afford 0.16 g of 1-(2-(4-((2,3-dihydro-1,4-benzodioxin-6-ylmethyl)amino)piperidin-1-yl)ethyl)quinoxalin-2(1H)-one hydrochloride as a red-brown solid.

Workup

  1. additionwas added at room temperature
  2. customthe solvent was removed under reduced pressure
  3. customTo the residue thus obtained
  4. filtrationthe resulting solid was filtered

Sources & evidence

ORD record
ord-f7fb7e5b5df14693b0212db7b0dd34bf
Source dataset
uspto-grants-2013_09
Patent number
US08524738B2

Reaction notes

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