Piperazine → HCID 22167853, compound

HRID 1031495Notes

Reaction equation

HRID 1031495 reaction equation
[NH:1]1[CH2:6][CH2:5][NH:4][CH2:3][CH2:2]1.Br[C:8]1[C:13]([O:14][CH3:15])=[CH:12][C:11]([Cl:16])=[CH:10][N:9]=1>O>[Cl:16][C:11]1[CH:12]=[C:13]([O:14][CH3:15])[C:8]([N:1]2[CH2:6][CH2:5][NH:4][CH2:3][CH2:2]2)=[N:9][CH:10]=1

Participants

4

Reactant 2

HCID 4837PiperazineHCID 190814342-Bromo-5-chloro-3-methoxypyridine

Product 1

HCID 22167853HCID 22167853, compoundYield 33%

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

Anhydrous piperazine (13.41 g) and 2-bromo-5-chloro-3-methoxypridine (3.50 g) were heated in an autoclave at 100° C. for 20 h. The mixture was dissolved in water (10 mL) and extracted with CH2Cl2 (3×100 mL). The combined organic extracts were washed with a saturated NaCl soution, dried with K2CO3, filtered and concentrated under reduced pressure. Silica gel chromatography (CH2Cl2 /MeOH; 90:10) of the residue yielded product (1.17 g, 33%).

Workup

  1. extractionextracted with CH2Cl2 (3×100 mL)
  2. washThe combined organic extracts were washed with a saturated NaCl soution
  3. dry with materialdried with K2CO3
  4. filtrationfiltered
  5. concentrationconcentrated under reduced pressure

Sources & evidence

ORD record
ord-05dc1621ca974f18932cfde077473ec6
Source dataset
uspto-grants-1990_09
Patent number
US04954502

Reaction notes

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