Phosphoric Acid → HCID 9948054, compound

HRID 2380211Notes

Reaction equation

HRID 2380211 reaction equation
[N:1]1[C:6](=O)[CH2:5][CH2:4][N:3]2[CH:8]=[CH:9][CH:10]=[CH:11][C:2]=12.O[P:13]([OH:16])([OH:15])=[O:14].P(Cl)(Cl)Cl>Cl>[N:1]1[C:6]([P:13]([OH:16])(=[O:14])[OH:15])([P:13]([OH:16])(=[O:14])[OH:15])[CH2:5][CH2:4][N:3]2[CH:8]=[CH:9][CH:10]=[CH:11][C:2]=12

Participants

5

Reactant 3

HCID 1004Phosphoric AcidHCID 24387Phosphorus trichlorideHCID 795003,4-Dihydro-2H-pyrido(1,2-a)pyrimidin-2-one

Product 1

HCID 9948054HCID 9948054, compound

Reagents, catalysts & solvents 1

HCID 313Hydrochloric AcidSolvent

Conditions

Temperature
100 °C

Procedure

5 g 3,4-Dihydropyrido-(1,2-a)-pyrimidin-2-one (Fluka) were melted at 80° C. with 5.5 g H3PO4 and mixed, while stirring, with 5.9 ml PCl3. After 20 hours at the given temperature, it was mixed with 70 ml 2N HCl, stirred for 8 hours at 100° C. and, after cooling, filtered off from the undissolved part. The filtrate was evaporated on a rotary evaporator and purified by ion exchanger chromatography on Amberlite IR 120 (H+ form) with water as eluent. The fractions obtained after electrophoresis were evaporated in a vacuum and the oil remaining behind, after dissolving in a little water, brought to crystallisation by the addition of acetone.

Workup

  1. additionmixed
  2. temperatureafter cooling
  3. filtrationfiltered off from the undissolved part
  4. customThe filtrate was evaporated on a rotary evaporator
  5. custompurified by ion exchanger chromatography on Amberlite IR 120 (H+ form) with water as eluent
  6. customThe fractions obtained after electrophoresis
  7. customwere evaporated in a vacuum
  8. dissolutionafter dissolving in a little water
  9. custombrought to crystallisation by the addition of acetone

Sources & evidence

ORD record
ord-d0c17a9469564c4e942518a3886b630a
Source dataset
uspto-grants-1994_11
Patent number
US05366969

Reaction notes

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