Sodium periodate → HCID 20373041, compound

HRID 258541Notes

Reaction equation

HRID 258541 reaction equation
[CH3:1][S:2][C:3]1[CH:4]=[CH:5][C:6]2[N:12]3[C:13](=[O:16])[N:14]=[N:15][C:11]3=[CH:10][C:9](=[O:17])[N:8]([C:18]3[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=3)[C:7]=2[CH:24]=1.I([O-])(=O)(=O)=[O:26].[Na+]>CO>[CH3:1][S:2]([C:3]1[CH:4]=[CH:5][C:6]2[N:12]3[C:13](=[O:16])[N:14]=[N:15][C:11]3=[CH:10][C:9](=[O:17])[N:8]([C:18]3[CH:19]=[CH:20][CH:21]=[CH:22][CH:23]=3)[C:7]=2[CH:24]=1)=[O:26]

Participants

4

Reactant 2

HCID 23667635Sodium periodateHCID 70622601HCID 70622601, compound

Product 1

HCID 20373041HCID 20373041, compound

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

3.22 g of 8-(methylthio)-6-phenyl-1H-s-triazolo [4,3-a] [1,5]benzodiazepine-1,5 -dione and 2.14 g of sodium metaperiodate in 500 ml methanol is stirred at +5° C. for 24 hours. The reaction is evaporated; the residue dissolved in methylene chloride, washed with water, dried and concentrated. The concentrate is chromotographed on twenty silica gel (1000μ plates, 20× 20 cm) using acetone-methanol (9:1) as eluting solvent. the band containing the product is removed, stirred with acetone-methanol (4:1) and the silica gel filtered off. The filtrate is evaporated to give the title compound.

Workup

  1. customThe reaction is evaporated
  2. dissolutionthe residue dissolved in methylene chloride
  3. washwashed with water
  4. customdried
  5. concentrationconcentrated
  6. washas eluting solvent
  7. additionthe band containing the product
  8. customis removed
  9. filtrationthe silica gel filtered off
  10. customThe filtrate is evaporated

Sources & evidence

ORD record
ord-4235ccaf0fce47af9aa45f6464c86e0b
Source dataset
uspto-grants-1977_07
Patent number
US04033947

Reaction notes

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