1-Methylhomopiperazine → HCID 54934279, compound

HRID 2094248Notes

Reaction equation

HRID 2094248 reaction equation
F[C:2]1[CH:9]=[CH:8][C:5]([C:6]#[N:7])=[CH:4][C:3]=1[CH3:10].[CH3:11][N:12]1[CH2:18][CH2:17][CH2:16][NH:15][CH2:14][CH2:13]1>>[CH3:10][C:3]1[CH:4]=[C:5]([CH:8]=[CH:9][C:2]=1[N:15]1[CH2:16][CH2:17][CH2:18][N:12]([CH3:11])[CH2:13][CH2:14]1)[C:6]#[N:7]

Participants

3

Reactant 2

HCID 2283491-MethylhomopiperazineHCID 27791804-Fluoro-3-methylbenzonitrile

Product 1

HCID 54934279HCID 54934279, compound

Procedure

7.00 g (51.8 mmol) 4-fluoro-3-methyl-benzonitrile are heated to 110° C. together with 1-N-methyl-[1,4]diazepan for 1 week with stirring. After evaporation i. vac. the residue is separated on aluminium oxide (eluant: dichloromethane) and the corresponding fractions are again purified on silica gel (eluting gradient: dichloromethane/methanol 100:1->9:1).

Workup

  1. customAfter evaporation i
  2. customthe residue is separated on aluminium oxide (eluant: dichloromethane)
  3. customthe corresponding fractions are again purified on silica gel (eluting gradient: dichloromethane/methanol 100:1->9:1)

Sources & evidence

ORD record
ord-df787ef52b154a5f82f4987ec42b9ecb
Source dataset
uspto-grants-2013_05
Patent number
US08445525B2

Reaction notes

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