Hydrogen chloride-ethyl acetate → HCID 67539033, compound

HRID 2193188Notes

Reaction equation

HRID 2193188 reaction equation
[CH3:1][NH:2][C:3]([C:5]1[C:14]2[C:9](=[CH:10][CH:11]=[CH:12][CH:13]=2)[N:8]([CH2:15][CH2:16][N:17]2[CH2:22][CH2:21][CH:20]([NH:23][CH2:24][C:25]3[CH:29]=[C:28]([C:30]4[S:31][CH:32]=[CH:33][CH:34]=4)[O:27][N:26]=3)[CH2:19][CH2:18]2)[C:7](=[O:35])[CH:6]=1)=[O:4].[ClH:36].C(OCC)(=O)C>C(OCC)(=O)C>[ClH:36].[CH3:1][NH:2][C:3]([C:5]1[C:14]2[C:9](=[CH:10][CH:11]=[CH:12][CH:13]=2)[N:8]([CH2:15][CH2:16][N:17]2[CH2:22][CH2:21][CH:20]([NH:23][CH2:24][C:25]3[CH:29]=[C:28]([C:30]4[S:31][CH:32]=[CH:33][CH:34]=4)[O:27][N:26]=3)[CH2:19][CH2:18]2)[C:7](=[O:35])[CH:6]=1)=[O:4]

Participants

4

Reactant 2

HCID 21866389Hydrogen chloride-ethyl acetateHCID 59398318HCID 59398318, compound

Product 1

HCID 67539033HCID 67539033, compound

Reagents, catalysts & solvents 1

HCID 8857Ethyl AcetateSolvent2×

Procedure

To 2.0 mL of ethyl acetate solution containing 25 mg of N-methyl-2-oxo-1-(2-(4-(((5-(2-thienyl)isooxazol-3-yl)methyl)amino)piperidin-1-yl)ethyl)-1,2-dihydroquinoline-4-carboxamide, 0.5 mL of 4.0 mol/L hydrogen chloride/ethyl acetate solution was added under ice-cooling. 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, the resulting solid was filtered to give 23 mg of N-methyl-2-oxo-1-(2-(4-(((5-(2-thienyl)isooxazol-3-yl)methyl)amino)piperidin-1-yl)ethyl)-1,2-dihydroquinoline-4-carboxamide hydrochloride as a light brown solid.

Workup

  1. additionwas added under ice-
  2. temperaturecooling
  3. customthe solvent was removed under reduced pressure
  4. customTo the residue thus obtained
  5. filtrationthe resulting solid was filtered

Sources & evidence

ORD record
ord-32a647799aee43d6998218dadfb628c5
Source dataset
uspto-grants-2012_12
Patent number
US08329694B2

Reaction notes

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