Hydrochloric Acid → HCID 131735717, compound

HRID 2201394Notes

Reaction equation

HRID 2201394 reaction equation
[CH3:1][O:2][CH2:3][CH2:4][O:5][CH2:6][CH2:7][O:8][C:9]1[N:14]=[C:13]([NH2:15])[N:12]=[C:11]([NH2:16])[C:10]=1[N:17]=O.[ClH:19]>[Pd].C(O)C>[ClH:19].[ClH:19].[CH3:1][O:2][CH2:3][CH2:4][O:5][CH2:6][CH2:7][O:8][C:9]1[N:14]=[C:13]([NH2:15])[N:12]=[C:11]([NH2:16])[C:10]=1[NH2:17]

Participants

5

Reactant 2

HCID 313Hydrochloric AcidHCID 117870578HCID 117870578, compound

Product 1

HCID 131735717HCID 131735717, compoundYield 84.1%

Reagents, catalysts & solvents 2

HCID 23938PalladiumCatalystHCID 702EthanolSolvent

Procedure

1.5 g (0.04 mol %) of palladium on carbon (5%) was added to a solution of 11.3 g (0.044 mol) of 6-[2-(2-methoxyethoxyl)ethoxy]-5-nitrosopyrimidine-2,4-diamine from step 5.2 in 400 ml of ethanol, and shaking was performed at room temperature for 16 h under hydrogen-1 atmosphere. Then the reaction mixture was poured into 80 ml of diluted hydrochloric acid (0.23 mol), the catalyst was filtered off, and the filtrate was concentrated almost to dryness. The precipitated crystals were sucked off and post-washed with ethanol. 6-[2-(2-methoxyethoxyl)ethoxy]pyrimidine-2,4,5-triamine, dihydrochloride (11.7 g, 84%) was obtained as white crystals.

Workup

  1. filtrationthe catalyst was filtered off
  2. concentrationthe filtrate was concentrated almost to dryness
  3. washpost-washed with ethanol

Sources & evidence

ORD record
ord-025938ccbd794ad1b45d501441c0c6c3
Source dataset
uspto-grants-2016_06
Patent number
US09364408B2

Reaction notes

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