Sulfuric Acid → HCID 136398804, compound

HRID 261081Notes

Reaction equation

HRID 261081 reaction equation
[NH2:1][C:2]1[N:3]([CH2:16][CH2:17]O)[N:4]=[C:5]2[C:10]=1[C:9](=[O:11])[NH:8][C:7]([C:12]([CH3:15])([CH3:14])[CH3:13])=[N:6]2.[S:19](=O)(=[O:22])([OH:21])[OH:20]>>[NH2:1][C:2]1[N:3]([CH2:16][CH2:17][S:19]([OH:22])(=[O:21])=[O:20])[N:4]=[C:5]2[C:10]=1[C:9](=[O:11])[NH:8][C:7]([C:12]([CH3:15])([CH3:14])[CH3:13])=[N:6]2

Participants

3

Reactant 2

HCID 1118Sulfuric AcidHCID 135702348HCID 135702348, compound

Product 1

HCID 136398804HCID 136398804, compound

Procedure

3-Amino-2-(2-hydroxyethyl)-6-(1,1-dimethylethyl)-2,5-dihydropyrazolo[3,4-d]pyrimidin-4-one (5 g) prepared as in Example 52 was added to concentrated sulphuric acid (10 ml). The solution was kept at 130°-135° C. for 3 hours, then cooled and poured onto ice (30 g). The precipitate which formed was filtered off, water washed and dissolved in 2 M sodium hydroxide solution. A trace of solid was filtered off, and the filtrate was acidified with concentrated hydrochloric acid to re-precipitate the title compound (4.4 g), m.p. 307°-309° C. decomp.

Workup

  1. temperaturecooled
  2. additionpoured onto ice (30 g)
  3. customThe precipitate which formed
  4. filtrationwas filtered off
  5. washwater washed
  6. dissolutiondissolved in 2 M sodium hydroxide solution
  7. filtrationA trace of solid was filtered off

Sources & evidence

ORD record
ord-767f798a8b0b460b826f9461c7ec1055
Source dataset
uspto-grants-1979_08
Patent number
US04163846

Reaction notes

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