Dichloromethane → HCID 131728712, compound

HRID 1366568Notes

Reaction equation

HRID 1366568 reaction equation
[CH3:1][N:2]1[CH2:7][CH2:6][N:5](C(OC(C)(C)C)=O)[C@@H:4]([CH:15]([CH3:17])[CH3:16])[CH2:3]1.C(Cl)[Cl:19]>CO.Cl.O1CCOCC1>[ClH:19].[ClH:19].[CH3:1][N:2]1[CH2:7][CH2:6][NH:5][C@@H:4]([CH:15]([CH3:17])[CH3:16])[CH2:3]1

Participants

6

Reactant 2

HCID 6344DichloromethaneHCID 66936264HCID 66936264, compound

Product 1

HCID 131728712HCID 131728712, compound

Reagents, catalysts & solvents 3

HCID 313Hydrochloric AcidSolvent2×HCID 887MethanolSolvent2×HCID 312751,4-DioxaneSolvent2×

Procedure

1,1-Dimethylethyl (2S)-4-methyl-2-(1-methylethyl)-1-piperazinecarboxylate (2.18 g crude, 8.76 assumed mmol) was dissolved in a mixture of MeOH (5 mL), CH2Cl2 (5 mL), and 4 N HCl in dioxane (8 mL). After stirring overnight at room temperature, another 8 mL of 4 N HCl in dioxane and 8 mL of MeOH were added, which dissolved the white precipitate that had formed and pushed the reaction to completion. Evaporation of the solvents in vacuo provided (3S)-1-methyl-3-(1-methylethyl)piperazine, dihydrochloride (1.97 g) as a white solid.

Workup

  1. dissolutionwhich dissolved the white precipitate that
  2. customhad formed
  3. customthe reaction to completion
  4. customEvaporation of the solvents in vacuo

Sources & evidence

ORD record
ord-677e834e53c840728793b27a9b3d83dc
Source dataset
uspto-grants-2011_02
Patent number
US07893056B2

Reaction notes

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