HCID 66936334, compound → HCID 55288067, compound

HRID 1366648Notes

Reaction equation

HRID 1366648 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 66936334HCID 66936334, compound

Product 1

HCID 55288067HCID 55288067, compoundYield 100%

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

(2R,5R)-1,2,5-Trimethyl-4-(phenylmethyl)piperazine (680 mg, 3.11 mmol) was dissolved in 50 mL of MeOH, degassed and placed under argon. 10% Pd/C (170 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 6.5 mL 1N HCl was added, the resulting filtrate was concentrated in vacuo to provide the hydrochloride salt of (2R,5R)-1,2,5-trimethylpiperazine (251 mg, 100%). LCMS: (M+H)+: 129.1.

Workup

  1. customdegassed
  2. addition10% Pd/C (170 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 6.5 mL 1N HCl was added
  9. concentrationthe resulting filtrate was concentrated in vacuo

Sources & evidence

ORD record
ord-0025c7cdb0af4412abb76d77aa9f27b8
Source dataset
uspto-grants-2011_02
Patent number
US07893056B2

Reaction notes

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