Hydrochloride methanol → HCID 67740613, compound

HRID 741715Notes

Reaction equation

HRID 741715 reaction equation
[CH3:1][O:2][C:3](=[O:17])[C@H:4]([CH2:6][N:7]1[CH:11]=[CH:10][N:9]=[C:8]1[N:12]=CN(C)C)[NH2:5].[ClH:18].CO>>[ClH:18].[ClH:18].[CH3:1][O:2][C:3](=[O:17])[C@H:4]([CH2:6][N:7]1[CH:11]=[CH:10][N:9]=[C:8]1[NH2:12])[NH2:5]

Participants

3

Reactant 2

HCID 21893726Hydrochloride methanolHCID 54454034HCID 54454034, compound

Product 1

HCID 67740613HCID 67740613, compound

Conditions

Temperature
55 °C

Procedure

3-(2-Dimethylaminomethyleneaminoimidazol-1-yl)-L-alanine methyl ester (470 mg) was suspended in 20% hydrochloric acid-methanol (40 ml), and the suspension was stirred at 55° C. for 6 days. The solvent was evaporated under reduced pressure, methanol was added to the residue, and the solvent was evaporated again. Methanol-ether was added to the residue, and the mixture was allowed to stand to precipitate colorless needles. The crystals were separated by filtration, washed with methanol followed by ether, and dried to give the title compound (292 mg).

Workup

  1. customThe solvent was evaporated under reduced pressure, methanol
  2. additionwas added to the residue
  3. customthe solvent was evaporated again
  4. additionMethanol-ether was added to the residue
  5. customto precipitate colorless needles
  6. customThe crystals were separated by filtration
  7. washwashed with methanol
  8. customdried

Sources & evidence

ORD record
ord-00337ca28a5a4e80a88cbf6004f4c1e9
Source dataset
uspto-grants-1996_09
Patent number
US05552427

Reaction notes

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