Benzoyl Peroxide → HCID 178456479, compound

HRID 1086833Notes

Reaction equation

HRID 1086833 reaction equation
[CH2:1]([N:8]1[C:13]2=[N:14][N:15]3[CH2:19][CH2:18][NH:17][C:16]3=[C:12]2[C:11](=[O:20])[N:10]([CH2:21][CH2:22][CH3:23])[C:9]1=[O:24])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C(OOC(=O)C1C=CC=CC=1)(=O)C1C=CC=CC=1>C(Cl)(Cl)Cl>[CH2:1]([N:8]1[C:13]2=[N:14][N:15]3[CH:19]=[CH:18][NH:17][C:16]3=[C:12]2[C:11](=[O:20])[N:10]([CH2:21][CH2:22][CH3:23])[C:9]1=[O:24])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

Participants

4

Reactant 2

HCID 7187Benzoyl PeroxideHCID 135778496HCID 135778496, compound

Product 1

HCID 178456479HCID 178456479, compound

Reagents, catalysts & solvents 1

HCID 6212ChloroformSolvent

Procedure

A solution of 1-benzyl-3-propyl-1,2,3,4,6,7-hexahydro-5H-imidazo [2',1': 5,1]- pyrazolo[3,4-d]pyrimidine-2,4-dione (4.5 g) and benzoyl peroxide (5.0 g) in chloroform (100 ml) was refluxed for 18 hours. The reaction mixture was concentrated to dryness, and the residue was dissolved in chloroform. The solution was washed with an aqueous solution of sodium carbonate and water, followed by drying and concentration to dryness. The residue was purified by flash chromatography. Recrystallization of thus obtained crystals from methylene chloride/hexane afforded colorless crystals (2.3 g, 52%), m.p. 290°-292° C.

Workup

  1. concentrationThe reaction mixture was concentrated to dryness
  2. dissolutionthe residue was dissolved in chloroform
  3. washThe solution was washed with an aqueous solution of sodium carbonate and water
  4. customby drying
  5. concentrationconcentration to dryness
  6. customThe residue was purified by flash chromatography
  7. customRecrystallization of thus obtained crystals from methylene chloride/hexane afforded colorless crystals (2.3 g, 52%), m.p. 290°-292° C.

Sources & evidence

ORD record
ord-7433ddf0ea3b48338758c26681478436
Source dataset
uspto-grants-1991_07
Patent number
US05032594

Reaction notes

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