1-Methylpiperazine → HCID 89650357, compound

HRID 1479087Notes

Reaction equation

HRID 1479087 reaction equation
[CH3:1][N:2]1[CH2:7][CH2:6][NH:5][CH2:4][CH2:3]1.C(O[C:11](=[O:16])[C:12]([Br:15])([F:14])[F:13])C>C1COCC1>[Br:15][C:12]([F:13])([F:14])[C:11]([N:5]1[CH2:6][CH2:7][N:2]([CH3:1])[CH2:3][CH2:4]1)=[O:16]

Participants

4

Reactant 2

HCID 531671-MethylpiperazineHCID 69585Ethyl bromodifluoroacetate

Product 1

HCID 89650357HCID 89650357, compoundYield 71.2%

Reagents, catalysts & solvents 1

HCID 8028TetrahydrofuranSolvent

Procedure

1-Methyl-piperazine (1.23 g; 12.3 mmol; 5 eq.) was added to a solution of bromo-difluoro-acetic acid ethyl ester (500 mg; 2.46 mmol; 1 eq.) in THF (50 mL) and the reaction mixture was stirred at room temperature for 16 hours then concentrated in vacuo. The residue was taken up in EA, washed with water, dried over magnesium sulfate and concentrated in vacuo to afford the title compound (450 mg, 71%) as a yellow oil.

Workup

  1. concentrationthen concentrated in vacuo
  2. washwashed with water
  3. dry with materialdried over magnesium sulfate
  4. concentrationconcentrated in vacuo

Sources & evidence

ORD record
ord-8aa0ca2ec6594122b427cb195c96a3fb
Source dataset
uspto-grants-2016_08
Patent number
US09403835B2

Reaction notes

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