Hydrochloric Acid → 120241-23-8

HRID 1600440Notes

Reaction equation

HRID 1600440 reaction equation
[CH3:1][N:2]1[N:6]=[N:5][C:4]([C:7]2[CH:8]=[N:9][CH:10]=[CH:11][CH:12]=2)=[N:3]1.[ClH:13]>CC(C)=O.CCOCC>[ClH:13].[CH3:1][N:2]1[N:6]=[N:5][C:4]([CH:7]2[CH2:12][CH2:11][CH2:10][NH:9][CH2:8]2)=[N:3]1

Participants

5

Reactant 2

HCID 313Hydrochloric AcidHCID 19612501HCID 19612501, compound

Product 1

HCID 131716106120241-23-8Yield 26%

Reagents, catalysts & solvents 2

HCID 180AcetoneSolventHCID 3283Diethyl EtherSolvent

Procedure

To a solution of 12 (1.93 g, 0.012 mol) in acetone (50 ml) was added hydrogen chloride in ether until acidic reaction. The precipitate was filtered off, dried, and dissolved in methanol (25 ml). 5% palladium on charcoal (0.6 g) was added, and the mixture was shaked overnight under 3 atm. of hydrogen pressure. The catalyst was filtered off and the filtrate was evaporated to dryness. Crystallization from ethanol yielded 0.63 g (0.0031 mol, 26%) of title product M.P. 168°-172° C. Anal. (C7H14ClN5) C, H, N.

Workup

  1. customuntil acidic reaction
  2. filtrationThe precipitate was filtered off
  3. customdried
  4. dissolutiondissolved in methanol (25 ml)
  5. addition5% palladium on charcoal (0.6 g) was added
  6. filtrationThe catalyst was filtered off
  7. customthe filtrate was evaporated to dryness
  8. customCrystallization from ethanol

Sources & evidence

ORD record
ord-60edf243ccb0493086a32b0c8e78a6a2
Source dataset
uspto-grants-1999_11
Patent number
USRE036374

Reaction notes

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