Acetone → HCID 22711430, compound

HRID 1061008Notes

Reaction equation

HRID 1061008 reaction equation
Cl.C(O)C.CC(C)=O.C(OC([N:16]1[CH2:21][CH2:20][N:19]([C:22]([C:24]2[CH:29]=[CH:28][C:27]([C:30]3[CH:35]=[CH:34][CH:33]=[CH:32][N+:31]=3[O-:36])=[CH:26][CH:25]=2)=[O:23])[CH2:18][CH2:17]1)=O)(C)(C)C>ClCCl>[N:19]1([C:22]([C:24]2[CH:29]=[CH:28][C:27]([C:30]3[CH:35]=[CH:34][CH:33]=[CH:32][N+:31]=3[O-:36])=[CH:26][CH:25]=2)=[O:23])[CH2:20][CH2:21][NH:16][CH2:17][CH2:18]1

Participants

5

Reactant 3

HCID 180AcetoneHCID 21887872Ethanol hydrochlorideHCID 69700183HCID 69700183, compound

Product 1

HCID 22711430HCID 22711430, compound

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Procedure

In dichloromethane (2.5 ml), 2-[4-[[4-(tert-butoxycarbonyl)piperazin-1-yl]carbonyl]phenyl]pyridine N-oxide was dissolved. To the resulting solution, a saturated solution of ethanol hydrochloride (2.5 ml) was added, followed by stirring at room temperature for 1 hour. After the solvent was distilled off under reduced pressure, water was added to the residue, whereby an aqueous solution was obtained. Acetone was added to the aqueous solution until the solution became turbid. The precipitate was collected by filtration and washed with acetone, whereby the title compound (274 mg, 81%) was obtained.

Workup

  1. distillationAfter the solvent was distilled off under reduced pressure, water
  2. additionwas added to the residue, whereby an aqueous solution
  3. customwas obtained
  4. filtrationThe precipitate was collected by filtration
  5. washwashed with acetone, whereby the title compound (274 mg, 81%)
  6. customwas obtained

Sources & evidence

ORD record
ord-b5f09648e6234f70b2646c5849bad27f
Source dataset
uspto-grants-2003_02
Patent number
US06525042B1

Reaction notes

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