Phosphoric Acid → 6-[2-(1-Pyrrolidinyl)ethylamino]-7,8,9,10-tetrahydro-1,2,4-triazolo[3,4-a]phthalazine diphosphate

HRID 1154017Notes

Reaction equation

HRID 1154017 reaction equation
[N:1]1([CH2:6][CH2:7][NH:8][C:9]2[C:18]3[CH2:17][CH2:16][CH2:15][CH2:14][C:13]=3[C:12]3=[N:19][N:20]=[CH:21][N:11]3[N:10]=2)[CH2:5][CH2:4][CH2:3][CH2:2]1.[P:22](=[O:26])([OH:25])([OH:24])[OH:23]>C(O)C>[OH:26][P:22]([O:25][P:22]([OH:25])([OH:24])=[O:23])(=[O:24])[OH:23].[N:1]1([CH2:6][CH2:7][NH:8][C:9]2[C:18]3[CH2:17][CH2:16][CH2:15][CH2:14][C:13]=3[C:12]3=[N:19][N:20]=[CH:21][N:11]3[N:10]=2)[CH2:2][CH2:3][CH2:4][CH2:5]1

Participants

4

Reactant 2

HCID 1004Phosphoric AcidHCID 133655886-[2-(1-Pyrrolidinyl)ethylamino]-7,8,9,10-tetrahydro-1,2,4-triazolo[3,4-a]phthalazine

Product 1

HCID 867397886-[2-(1-Pyrrolidinyl)ethylamino]-7,8,9,10-tetrahydro-1,2,4-triazolo[3,4-a]phthalazine diphosphate

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent2×

Procedure

To a refluxing solution of 15.0 g of 6-[2-(1-pyrrolidinyl)ethylamino]-7,8,9,10-tetrahydro-1,2,4-triazolo[3,4-a]phthalazine in 45 ml of ethanol was slowly added a solution of 13.2 g of phosphoric acid in an equal volume of ethanol. An exothermic reaction with vigorous foaming took place. The resulting slurry was refluxed for 1 hour and then cooled. The solid was separated by filtration, washed with ethanol and with absolute ethanol, and then dried at 50° C. under reduced pressure to give 6-[2-(1-pyrrolidinyl)ethylamino]-7,8,9,10-tetrahydro-1,2,4-triazolo[3,4-a]phthalazine diphosphate.

Workup

  1. customAn exothermic reaction with vigorous foaming
  2. temperatureThe resulting slurry was refluxed for 1 hour
  3. temperaturecooled
  4. customThe solid was separated by filtration
  5. washwashed with ethanol and with absolute ethanol
  6. customdried at 50° C. under reduced pressure

Sources & evidence

ORD record
ord-7cadd7ac46a243d591f2fbac3e767b8d
Source dataset
uspto-grants-1984_12
Patent number
US04487930

Reaction notes

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