Sodium Carbonate → HCID 19994828, compound

HRID 1110379Notes

Reaction equation

HRID 1110379 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 2propanone were added dropwise 16.28 parts of 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-7849f8476f6646c8b6a6589c036dbe82
Source dataset
uspto-grants-1990_12
Patent number
US04975439

Reaction notes

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