Hydrochloric Acid → HCID 10392378, compound

HRID 1033115Notes

Reaction equation

HRID 1033115 reaction equation
[CH2:1]([C:5]1[N:6]([CH2:29][C:30]2[CH:39]=[CH:38][C:33]([C:34]([O:36]C)=[O:35])=[CH:32][CH:31]=2)[C:7](/[CH:10]=[C:11]2\[N:12]([CH2:22][C:23]3[N:24]=[C:25]([CH3:28])[S:26][CH:27]=3)[C:13](=[O:21])[N:14]([CH2:17][CH2:18][CH2:19][CH3:20])[C:15]\2=[O:16])=[CH:8][N:9]=1)[CH2:2][CH2:3][CH3:4].Cl.C([O-])(=O)C.[Na+]>O>[CH2:1]([C:5]1[N:6]([CH2:29][C:30]2[CH:31]=[CH:32][C:33]([C:34]([OH:36])=[O:35])=[CH:38][CH:39]=2)[C:7](/[CH:10]=[C:11]2\[N:12]([CH2:22][C:23]3[N:24]=[C:25]([CH3:28])[S:26][CH:27]=3)[C:13](=[O:21])[N:14]([CH2:17][CH2:18][CH2:19][CH3:20])[C:15]\2=[O:16])=[CH:8][N:9]=1)[CH2:2][CH2:3][CH3:4]

Participants

5

Procedure

A mixture of methyl Z-4-[[2-butyl-5-[[1-butyl-3-[(2-methyl-4-thiazolyl)methyl]-2,5-dioxo-4-imidazolidinylidene]methyl]-1H-imidazol-1-yl]methyl]benzoate (0.428 g, 0.65 mmol) and 2N HCl (12 mL) is refluxed for 1 hour in which time all the solid dissolved. Solvents are removed in vacuo and the mixture is evaporated from ethanol (5 mL) three times. The solid that results is treated with 5% aqueous sodium acetate (10 mL) and water (10 mL) to precipitate a gummy solid which is dissolved in methylene chloride (30 mL). The organic layer is dried over Na2SO4 and then evaporated in vacuo. The residue is recrystallized from hot ethyl acetate/hexane.

Workup

  1. temperatureis refluxed for 1 hour in which time all the solid
  2. dissolutiondissolved
  3. customSolvents are removed in vacuo
  4. customthe mixture is evaporated from ethanol (5 mL) three times
  5. customThe solid that results
  6. customto precipitate a gummy solid which
  7. dissolutionis dissolved in methylene chloride (30 mL)
  8. dry with materialThe organic layer is dried over Na2SO4
  9. customevaporated in vacuo
  10. customThe residue is recrystallized from hot ethyl acetate/hexane

Sources & evidence

ORD record
ord-a10dc677012048e5970a461c351b7e4a
Source dataset
uspto-grants-1994_05
Patent number
US05308853

Reaction notes

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