Ethanol hydrochloride → HCID 178471179, compound

HRID 606455Notes

Reaction equation

HRID 606455 reaction equation
[NH:1]1[CH:5]=[N:4][C:3]([CH2:6][CH2:7][C:8]([OH:10])=[O:9])=[N:2]1.Cl.[CH2:12](O)[CH3:13]>C(O)C>[NH:1]1[CH:5]=[N:4][C:3]([CH2:6][CH2:7][C:8]([O:10][CH2:12][CH3:13])=[O:9])=[N:2]1

Participants

4

Reactant 2

HCID 21887872Ethanol hydrochlorideHCID 178525367HCID 178525367, compound

Product 1

HCID 178471179HCID 178471179, compoundYield 33%

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Conditions

Temperature
90 °C

Procedure

A suspension of 3-(1H-1,2,4-triazol-3-yl)propanoic acid obtained in Reference Example 22 (11.6 g, 3.54 mmol) and 2N hydrogen chloride/ethanol (100 mL) in ethanol (100 mL) was stirred at 90° C. for 15 hr. The insoluble material was filtered off, and the filtrate was concentrated under reduced pressure. The residue was extracted with ethyl acetate and water. The aqueous layer was neutralized with saturated aqueous sodium carbonate solution, and the organic layer was washed with saturated brine, dried over sodium sulfate, and concentrated to give the title compound as a yellow powder (4.36 g, 33%).

Workup

  1. filtrationThe insoluble material was filtered off
  2. concentrationthe filtrate was concentrated under reduced pressure
  3. extractionThe residue was extracted with ethyl acetate and water
  4. washthe organic layer was washed with saturated brine
  5. dry with materialdried over sodium sulfate
  6. concentrationconcentrated

Sources & evidence

ORD record
ord-1e0cf61ff4704e078fcb3878904fa107
Source dataset
uspto-grants-2011_03
Patent number
US07915267B2

Reaction notes

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