Hydrochloric Acid → HCID 178491370, compound

HRID 447941

Reaction equation

HRID 447941 reaction equation
Cl.[CH3:2][O:3][C:4]1[CH:11]=[CH:10][CH:9]=[C:8]([O:12][CH3:13])[C:5]=1[CH2:6][NH2:7].[N-:14]([C:17]#[N:18])[C:15]#[N:16].[Na+]>>[C:15]([NH:14][C:17]([NH:7][CH2:6][C:5]1[C:8]([O:12][CH3:13])=[CH:9][CH:10]=[CH:11][C:4]=1[O:3][CH3:2])=[NH:18])#[N:16]

Participants

4

Reactant 3

HCID 313Hydrochloric AcidHCID 28008722,6-DimethoxybenzylamineHCID 4350929Sodium dicyanamide

Product 1

HCID 178491370HCID 178491370, compound

Procedure

15 ml 2N hydrochloric acid were added to 5.0 g (29.9 mmol) 2,6-dimethoxybenzylamine and the aqueous phase was subsequently removed under vacuum. The residue was then dissolved in 50 ml 1-butanol and 2.66 g (29.9 mmol) of sodium dicyanamide were added. The reaction mixture was heated for 5.5 hours at reflux and stirred for 12 hours at room temperature. The precipitate formed was filtered off, was washed with diethylether; 6.81 g.

Workup

  1. customthe aqueous phase was subsequently removed under vacuum
  2. dissolutionThe residue was then dissolved in 50 ml 1-butanol
  3. temperatureThe reaction mixture was heated for 5.5 hours
  4. temperatureat reflux
  5. customThe precipitate formed
  6. filtrationwas filtered off
  7. washwas washed with diethylether

Sources & evidence

ORD record
ord-0740ffcdbd084f38a1576fed031345a4
Source dataset
uspto-grants-2013_07
Patent number
US08481576B2

Linked notes

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