Hydrochloric Acid → HCID 68843024, compound

HRID 1948617Notes

Reaction equation

HRID 1948617 reaction equation
Cl.[CH3:2][NH:3][C:4]1([C:14]2[N:15]([CH3:19])[N:16]=[CH:17][N:18]=2)[CH2:13][CH2:12][C:7]2(OCC[O:8]2)[CH2:6][CH2:5]1>CCOCC>[CH3:2][NH:3][C:4]1([C:14]2[N:15]([CH3:19])[N:16]=[CH:17][N:18]=2)[CH2:13][CH2:12][C:7](=[O:8])[CH2:6][CH2:5]1

Participants

4

Reactant 2

HCID 313Hydrochloric AcidHCID 68842365HCID 68842365, compound

Product 1

HCID 68843024HCID 68843024, compoundYield 83%

Reagents, catalysts & solvents 1

HCID 3283Diethyl EtherSolvent

Procedure

5% hydrochloric acid (330 ml) was added at room temperature to methyl-[8-(2-methyl-2H-[1,2,4]triazol-3-yl)-1,4-dioxaspiro[4.5]dec-8-yl]-amine (4.2 g, 16.646 mmole) and the mixture was stirred for 3 days at room temperature. Ether (120 ml) was added to the reaction mixture. The phases were separated. The aqueous phase was made alkaline with 5N NaOH and extracted with dichloromethane (4×50 ml). The organic phase was dried over sodium sulfate and concentrated by evaporation to dryness in vacuo. The product was obtained as a colourless crystalline solid in a yield of 83% (2.89 g, 13.862 mmole).

Workup

  1. customThe phases were separated
  2. extractionextracted with dichloromethane (4×50 ml)
  3. dry with materialThe organic phase was dried over sodium sulfate
  4. concentrationconcentrated by evaporation to dryness in vacuo
  5. customThe product was obtained as a colourless crystalline solid in a yield of 83% (2.89 g, 13.862 mmole)

Sources & evidence

ORD record
ord-a3f133fbf6ab485cbffc0c9b06774fc2
Source dataset
uspto-grants-2013_03
Patent number
US08399503B2

Reaction notes

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