Sodium Carbonate → HCID 19994828, compound

HRID 2248615Notes

Reaction equation

HRID 2248615 reaction equation
[CH3:1][CH:2]1[CH2:7][N:6]([CH2:8][C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)[CH2:5][CH2:4][NH:3]1.C(=O)([O-])[O-].[Na+].[Na+].[Cl:21][CH2:22][CH2:23][CH:24]([CH3:28])[C:25](Cl)=[O:26]>CC(=O)C>[ClH:21].[Cl:21][CH2:22][CH2:23][CH:24]([CH3:28])[C:25]([N:3]1[CH2:4][CH2:5][N:6]([CH2:8][C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)[CH2:7][CH:2]1[CH3:1])=[O:26]

Participants

5

Reactant 3

HCID 10340Sodium CarbonateHCID 27275201-Benzyl-3-methylpiperazineHCID 137705824-Chloro-2-methylbutanoyl chloride

Product 1

HCID 19994828HCID 19994828, compoundYield 45.5%

Reagents, catalysts & solvents 1

HCID 180AcetoneSolvent

Procedure

To a stirred mixture of 20 parts of 2-methyl-4-(phenylmethyl)piperazine, 11.13 parts of sodium carbonate and 120 parts of 2-propanone were added dropwise 16.28 parts of a 4-chloro-2-methylbutanoyl chloride. Upon completion, stirring was continued for 45 minutes. The precipitated product was filtered off and taken up in dichloromethane. Water and sodium carbonate were added. The organic layer was separated, dried, filtered and evaporated. The residue was converted into the hydrochloride salt in 2-propanol. The salt was filtered off and dried in vacuo at 40° C., yielding 16.5 parts (45.5%) of 1-(4-chloro-2-methyl-1-oxobutyl)-2-methyl-4-(phenylmethyl)piperazine monohydrochloride (int. 25).

Workup

  1. filtrationThe precipitated product was filtered off
  2. additionWater and sodium carbonate were added
  3. customThe organic layer was separated
  4. customdried
  5. filtrationfiltered
  6. customevaporated
  7. filtrationThe salt was filtered off
  8. customdried in vacuo at 40° C.

Sources & evidence

ORD record
ord-4ad249f7a4054602ac77500ca7f2ae13
Source dataset
uspto-grants-1991_08
Patent number
US05041454

Reaction notes

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