Hydrochloric Acid → HCID 57331533, compound

HRID 1844791Notes

Reaction equation

HRID 1844791 reaction equation
[C:1]([C:3]1[CH:8]=[CH:7][C:6]([C:9]([N:11]2[CH2:16][CH2:15][N:14]([CH3:17])[CH2:13][CH2:12]2)=[O:10])=[CH:5][C:4]=1[N+:18]([O-:20])=[O:19])#[CH:2].[ClH:21]>CO>[ClH:21].[C:1]([C:3]1[CH:8]=[CH:7][C:6]([C:9]([N:11]2[CH2:16][CH2:15][N:14]([CH3:17])[CH2:13][CH2:12]2)=[O:10])=[CH:5][C:4]=1[N+:18]([O-:20])=[O:19])#[CH:2]

Participants

4

Reactant 2

HCID 313Hydrochloric AcidHCID 57331530HCID 57331530, compound

Product 1

HCID 57331533HCID 57331533, compoundYield 54.1%

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

0.75 g (2.74 mmol) (4-ethynyl-3-nitrophenyl) (4-methylpiperazin-1-yl)ketone (Compound I-24) and 7.5 ml anhydrous methanol were added into a 50 ml single-neck flask, magnetically stirred to dissolve. The mixture was adjusted to a pH value of 2 by adding concentrated hydrochloric acid. A white solid was precipitated under cooling with ice water, and filtered. The filter cake was washed with anhydrous ethanol, dried to obtain 0.46 g (4-ethynyl-3-nitrophenyl) (4-methylpiperazin-1-yl)ketone hydrochloride (Compound I-29), yield: 54.1%.

Workup

  1. dissolutionto dissolve
  2. customA white solid was precipitated
  3. temperatureunder cooling with ice water
  4. filtrationfiltered
  5. washThe filter cake was washed with anhydrous ethanol
  6. customdried

Sources & evidence

ORD record
ord-19283c906b884db79129da101e71377d
Source dataset
uspto-grants-2015_02
Patent number
US08946478B2

Reaction notes

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