Ammonia → HCID 13607465, compound

HRID 568331Notes

Reaction equation

HRID 568331 reaction equation
[NH2:1][C:2]1[C:7]([NH2:8])=[C:6]([N:9]2[CH2:14][CH2:13][N:12]([CH3:15])[CH2:11][CH2:10]2)[N:5]=[CH:4][N:3]=1.[C:16](O)(=O)[C:17]1[CH:22]=[CH:21][N:20]=[CH:19][CH:18]=1.N>O>[CH3:15][N:12]1[CH2:13][CH2:14][N:9]([C:6]2[N:5]=[CH:4][N:3]=[C:2]3[C:7]=2[NH:8][C:16]([C:17]2[CH:22]=[CH:21][N:20]=[CH:19][CH:18]=2)=[N:1]3)[CH2:10][CH2:11]1

Participants

5

Reactant 3

HCID 222AmmoniaHCID 5922Isonicotinic AcidHCID 19137070HCID 19137070, compound

Product 1

HCID 13607465HCID 13607465, compoundYield 35.3%

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

A mixture of 3 g of 4,5-diamino-6-(4-methyl-1-piperazinyl) pyrimidine, 1.8 g of isonicotinic acid and 45 g of polyphosphoric acid is stirred at 160°-170° C. for 4 hours under nitrogen atmosphere. To the resultant mixture is added 200 ml of water and the solution is neutralized with an ammonia solution. The crystals precipitated are filtered and washed with water, and then recrystallized from methanol to give 1.5 g of 6-(4- methyl-1-piperazinyl)-8-(4-pyridyl)purine, melting at 333°-335° C.

Workup

  1. customThe crystals precipitated
  2. filtrationare filtered
  3. washwashed with water
  4. customrecrystallized from methanol

Sources & evidence

ORD record
ord-8ee110db3d704378897f3a482f326ffb
Source dataset
uspto-grants-1988_03
Patent number
US04728644

Reaction notes

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