Methylamine → HCID 21416643, compound

HRID 442113Notes

Reaction equation

HRID 442113 reaction equation
[CH3:1][N:2]1[C:6]2=[N:7][C:8](S)=[N:9][C:10](C)=[C:5]2[C:4]([C:13]2[O:14][C:15]([N+:18]([O-:20])=[O:19])=[CH:16][CH:17]=2)=[N:3]1.[CH3:21][NH2:22]>C(O)C.C(OCC)(=O)C>[CH3:21][NH:22][C:10]1[N:9]=[CH:8][N:7]=[C:6]2[N:2]([CH3:1])[N:3]=[C:4]([C:13]3[O:14][C:15]([N+:18]([O-:20])=[O:19])=[CH:16][CH:17]=3)[C:5]=12

Participants

5

Reactant 2

HCID 6329MethylamineHCID 178433546HCID 178433546, compound

Product 1

HCID 21416643HCID 21416643, compound

Reagents, catalysts & solvents 2

HCID 702EthanolSolventHCID 8857Ethyl AcetateSolvent

Procedure

A mixture of 3.0 grams of 1-methyl-4-methyl-mercapto-3-(5-nitro-2-furyl)-1H-pyrazolo [3,4-d] pyrimidine, 50 millitres of a 33% solution of methylamine in ethanol and 20 milliliters of ethyl acetate was heated at reflux for 1hour and cooled. The crystalline product formed was collected, washed with ethanol and dried. Recrystallisation from ehtyl acetate gave 4-methylamino-1-methyl-3-(5-nitro-2-furyl)-1H-pyrazolo [3,4-d]pyrimidine having melting point 280° C. identical to the product obtained in Example 13.

Workup

  1. temperaturewas heated
  2. temperatureat reflux for 1hour
  3. temperaturecooled
  4. customThe crystalline product formed
  5. customwas collected
  6. washwashed with ethanol
  7. customdried
  8. customRecrystallisation from ehtyl acetate

Sources & evidence

ORD record
ord-af9c4185f67c41b6b96a3db2f3d24387
Source dataset
uspto-grants-1977_08
Patent number
US04044130

Reaction notes

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