Ethylene Glycol → HCID 21291413, compound

HRID 622657Notes

Reaction equation

HRID 622657 reaction equation
[CH2:1]([O:3][C:4]([C:6]1[C:11]2[C:12](=[O:27])[N:13]([CH3:26])[CH2:14][C:15]3[N:16]([CH:17]=[N:18][C:19]=3[C:20]3[N:24]=[C:23]([CH3:25])[O:22][N:21]=3)[C:10]=2[CH:9]=[CH:8][CH:7]=1)=[O:5])[CH3:2].C(O)C[OH:30]>S(=O)(=O)(O)O>[OH:30][CH2:2][CH2:1][O:3][C:4]([C:6]1[C:11]2[C:12](=[O:27])[N:13]([CH3:26])[CH2:14][C:15]3[N:16]([CH:17]=[N:18][C:19]=3[C:20]3[N:24]=[C:23]([CH3:25])[O:22][N:21]=3)[C:10]=2[CH:9]=[CH:8][CH:7]=1)=[O:5]

Participants

4

Reactant 2

HCID 174Ethylene GlycolHCID 21291402HCID 21291402, compound

Product 1

HCID 21291413HCID 21291413, compound

Reagents, catalysts & solvents 1

HCID 1118Sulfuric AcidCatalyst

Conditions

Temperature
130 °C

Procedure

7-Ethoxycarbonyl-5,6-dihydro-5-methyl-3-(5-methyl-1,2,4-oxadiazol-3-yl)-6-oxo-4H-imidazo(1,5-a)(1,4)benzodiazepine (500 mg) was dissolved in ethylene glycol (20 ml) and 3 drops of concentrated sulphuric acid were added. The solution was then stirred at 130° C. for 24 hours, cooled and partitioned between water (150 ml) and CHCl3 (150 ml). The organic phase was separated, dried over Na2SO4, and evaporated to give the title compound as white crystals.

Workup

  1. temperaturecooled
  2. custompartitioned between water (150 ml) and CHCl3 (150 ml)
  3. customThe organic phase was separated
  4. dry with materialdried over Na2SO4
  5. customevaporated

Sources & evidence

ORD record
ord-daf41eada2e04ba681c6ccf11b874524
Source dataset
uspto-grants-1988_09
Patent number
US04772599

Reaction notes

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