Hydroxylamine → HCID 21548197, compound

HRID 442116Notes

Reaction equation

HRID 442116 reaction equation
[NH2:1][OH:2].CO.Cl[C:6]1[N:11]=[CH:10][N:9]=[C:8]2[N:12]([CH3:23])[N:13]=[C:14]([C:15]3[O:16][C:17]([N+:20]([O-:22])=[O:21])=[CH:18][CH:19]=3)[C:7]=12>C(O)C>[OH:2][NH:1][C:6]1[N:11]=[CH:10][N:9]=[C:8]2[N:12]([CH3:23])[N:13]=[C:14]([C:15]3[O:16][C:17]([N+:20]([O-:22])=[O:21])=[CH:18][CH:19]=3)[C:7]=12

Participants

5

Reactant 3

HCID 787HydroxylamineHCID 887MethanolHCID 21416630HCID 21416630, compound

Product 1

HCID 21548197HCID 21548197, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

A solution containing 0.7 grams of anhydrous hydroxylamine in 50 millilitres if methanol was added to a solution containing 1.4 grams of 4-chloro-1-methyl-3-(5-nitro-2-furyl)-1H-pyrazolo [3,4-d]pyrimidine dissolved in 600 millilitres of ethanol, at a temperature of 30° C. and the mixture was allowed to stand for 30 minutes at room temperature. The mixture was gently heated at reflux for a further 15 minutes and cooled. The crystalline product was washed with ether and dried. Recrystallisation from dimethylformamide gave 4-hydroxyamino-1-methyl-3-(5-nitro-2-furyl)-1H-pyrazolo [3,4-d] pyrimidine, having melting point 294° C.

Workup

  1. additionwas added to a solution
  2. temperatureThe mixture was gently heated
  3. temperatureat reflux for a further 15 minutes
  4. temperaturecooled
  5. washThe crystalline product was washed with ether
  6. customdried
  7. customRecrystallisation from dimethylformamide

Sources & evidence

ORD record
ord-dd97d222f9004c90a58389992a13ab0c
Source dataset
uspto-grants-1977_08
Patent number
US04044130

Reaction notes

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