Hydrochloric Acid → HCID 22716029, compound

HRID 1582928Notes

Reaction equation

HRID 1582928 reaction equation
[ClH:1].[NH2:2][CH2:3][C:4]1[N:8]([CH3:9])[N:7]=[C:6]([C:10]([NH2:12])=[O:11])[N:5]=1>C(OCC)(=O)C>[ClH:1].[NH2:2][CH2:3][C:4]1[N:8]([CH3:9])[N:7]=[C:6]([C:10]([NH2:12])=[O:11])[N:5]=1

Participants

4

Reactant 2

HCID 313Hydrochloric AcidHCID 227160095-(Aminomethyl)-1-methyl-1H-1,2,4-triazole-3-carboxamide

Product 1

HCID 22716029HCID 22716029, compound

Reagents, catalysts & solvents 1

HCID 8857Ethyl AcetateSolvent

Procedure

Hydrogen chloride was passed to saturation at 5° C. to a solution of 4.7 g (not more-than 18.4 mmol) of 5-aminomethyl-1-methyl-1H-[1,2,4]-triazole-3-carboxamide in 600 ml of ethyl acetate, during which process a white precipitate formed. The mixture was stirred overnight at room temperature and concentrated on a rotary evaporator, diethyl ether was added, the mixture was concentrated and again taken up in diethyl ether, and the precipitate was filtered off and dried. This gave 3.7 g of a white solid which still contained ammonium chloride. 1H NMR (270 MHz, DMSO-d6): δ=3.95 (s, 3H), 4.3 (bs, 2H), 7.6 (bs, 1H), 7.75 (bs, 1H), 8.7-8.9 (m, 2H).

Workup

  1. customsaturation at 5° C.
  2. customduring which process a white precipitate formed
  3. concentrationconcentrated on a rotary evaporator, diethyl ether
  4. additionwas added
  5. concentrationthe mixture was concentrated
  6. filtrationthe precipitate was filtered off
  7. customdried

Sources & evidence

ORD record
ord-f3fe6551de5947e99c3e23307ade7bd1
Source dataset
uspto-grants-2004_05
Patent number
US06740647B1

Reaction notes

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