Hydrogen chloride-ethyl acetate → HCID 67537667, compound

HRID 39963Notes

Reaction equation

HRID 39963 reaction equation
[C:1]1([C:7]#[C:8][CH2:9][N:10]([CH2:31][C:32]#[C:33][C:34]2[CH:39]=[CH:38][CH:37]=[CH:36][CH:35]=2)[CH:11]2[CH2:16][CH2:15][N:14]([CH2:17][CH2:18][N:19]3[C:28]4[C:23](=[CH:24][CH:25]=[C:26]([F:29])[CH:27]=4)[N:22]=[CH:21][C:20]3=[O:30])[CH2:13][CH2:12]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[ClH:40].C(OCC)(=O)C>C(Cl)(Cl)Cl>[ClH:40].[C:34]1([C:33]#[C:32][CH2:31][N:10]([CH2:9][C:8]#[C:7][C:1]2[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=2)[CH:11]2[CH2:16][CH2:15][N:14]([CH2:17][CH2:18][N:19]3[C:28]4[C:23](=[CH:24][CH:25]=[C:26]([F:29])[CH:27]=4)[N:22]=[CH:21][C:20]3=[O:30])[CH2:13][CH2:12]2)[CH:39]=[CH:38][CH:37]=[CH:36][CH:35]=1

Participants

4

Reactant 2

HCID 21866389Hydrogen chloride-ethyl acetateHCID 593983021-(2-(4-(bis(3-phenyl-2-propyn-1-yl)amino)piperidin-1-yl)ethyl)-7-fluoroquinoxalin-2(1H)-one

Product 1

HCID 67537667HCID 67537667, compound

Reagents, catalysts & solvents 1

HCID 6212ChloroformSolvent

Procedure

To 5 mL of a chloroform solution containing 132 mg of 1-(2-(4-(bis(3-phenyl-2-propyn-1-yl)amino)piperidin-1-yl)ethyl)-7-fluoroquinoxalin-2(1H)-one, 0.5 mL of 4 mol/L hydrogen chloride/ethyl acetate was added, and stirred at room temperature for 10 min. The solvent was removed under reduced pressure, ethyl acetate was added, and the resulting solid was filtered to give 141 mg of 1-(2-(4-(bis(3-phenyl-2-propyn-1-yl)amino)piperidin-1-yl)ethyl)-7-fluoroquinoxalin-2(1H)-one hydrochloride as a pale brown solid.

Workup

  1. additionwas added
  2. customThe solvent was removed under reduced pressure, ethyl acetate
  3. additionwas added
  4. filtrationthe resulting solid was filtered

Sources & evidence

ORD record
ord-909734bbe43f478ebf7f2169d2ef9646
Source dataset
uspto-grants-2013_09
Patent number
US08524738B2

Reaction notes

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