1-Methylpiperazine → Benzonitrile, 2-fluoro-6-(4-methyl-1-piperazinyl)-

HRID 2164447Notes

Reaction equation

HRID 2164447 reaction equation
F[C:2]1[CH:9]=[CH:8][CH:7]=[C:6]([F:10])[C:3]=1[C:4]#[N:5].[CH3:11][N:12]1[CH2:17][CH2:16][NH:15][CH2:14][CH2:13]1>>[F:10][C:6]1[CH:7]=[CH:8][CH:9]=[C:2]([N:15]2[CH2:16][CH2:17][N:12]([CH3:11])[CH2:13][CH2:14]2)[C:3]=1[C:4]#[N:5]

Participants

3

Reactant 2

HCID 531671-MethylpiperazineHCID 746952,6-Difluorobenzonitrile

Product 1

HCID 13469798Benzonitrile, 2-fluoro-6-(4-methyl-1-piperazinyl)-

Procedure

2,6-Difluorobenzonitrile is reacted with N-methyl piperazine following the procedure of Example 5. The reaction mixture is extracted with methylene chloride after addition of water. The methylene chloride is extracted with dilute HCl which is basified and extracted with methylene chloride. The resulting crude oil after evaporation is taken in ethanol and i-PrOH-HCl is added to give the title compound as the hydrochloride salt, 1.4 g m.p. 245°-247° C.

Workup

  1. extractionThe reaction mixture is extracted with methylene chloride
  2. additionafter addition of water
  3. extractionThe methylene chloride is extracted with dilute HCl which
  4. extractionextracted with methylene chloride
  5. customThe resulting crude oil after evaporation
  6. additioni-PrOH-HCl is added

Sources & evidence

ORD record
ord-36441a7207f94b70bfa19aaa507cb8ea
Source dataset
uspto-grants-1985_03
Patent number
US04504660

Reaction notes

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