HCID 66936064, compound → HCID 66936269, compound

HRID 1366677Notes

Reaction equation

HRID 1366677 reaction equation
[CH3:1][N:2]1[CH2:7][C@H:6]([CH3:8])[N:5](CC2C=CC=CC=2)[CH2:4][C@@H:3]1[CH3:16]>CO>[CH3:1][N:2]1[CH2:7][C@H:6]([CH3:8])[NH:5][CH2:4][C@@H:3]1[CH3:16]

Participants

3

Reactant 1

HCID 66936064HCID 66936064, compound

Product 1

HCID 66936269HCID 66936269, compoundYield 155.8%

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

(2S,5S)-1,2,5-Trimethyl-4-(phenylmethyl)piperazine (782 mg, 3.58 mmol) was dissolved in 50 mL of MeOH, degassed and placed under argon. 10% Pd/C (200 mg) was added, and the contents were thoroughly degassed and placed under a hydrogen balloon for approximately 3 hrs. The contents were then degassed and filtered through Celite, and the Celite pad was washed with DCM and MeOH. After 7.5 mL 1N HCl was added, the resulting filtrate was concentrated in vacuo to provide the hydrochloride salt of (2S,5S)-1,2,5-trimethylpiperazine (715 mg, 100%). LCMS: (M+H)+: 129.1.

Workup

  1. customdegassed
  2. addition10% Pd/C (200 mg) was added
  3. customthe contents were thoroughly degassed
  4. customfor approximately 3 hrs
  5. customThe contents were then degassed
  6. filtrationfiltered through Celite
  7. washthe Celite pad was washed with DCM and MeOH
  8. additionAfter 7.5 mL 1N HCl was added
  9. concentrationthe resulting filtrate was concentrated in vacuo

Sources & evidence

ORD record
ord-bf2199a4f08a470c87d448d0fa4fca80
Source dataset
uspto-grants-2011_02
Patent number
US07893056B2

Reaction notes

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