Phosphoric Acid → HCID 86653868, compound

HRID 1875700Notes

Reaction equation

HRID 1875700 reaction equation
[OH:1][CH2:2][C@H:3]1[CH2:7][CH2:6][CH2:5][N:4]1[CH2:8][CH2:9][C:10]1[NH:11][C:12](=[O:21])[C:13]2[C:18]([CH:19]=1)=[C:17]([CH3:20])[CH:16]=[CH:15][CH:14]=2.[P:22](=[O:26])([OH:25])([OH:24])[OH:23]>C(O)C>[OH2:1].[OH:26][P:22]([O:25][P:22]([OH:25])([OH:24])=[O:23])(=[O:24])[OH:23].[OH:1][CH2:2][C@H:3]1[CH2:7][CH2:6][CH2:5][N:4]1[CH2:8][CH2:9][C:10]1[NH:11][C:12](=[O:21])[C:13]2[C:18]([CH:19]=1)=[C:17]([CH3:20])[CH:16]=[CH:15][CH:14]=2

Participants

4

Reactant 2

HCID 1004Phosphoric Acid2×HCID 10424118(R)-3-(2-(2-(hydroxymethyl)pyrrolidin-1-yl)ethyl)-5-methylisoquinolin-1(2H)-one

Product 1

HCID 86653868HCID 86653868, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent2×

Procedure

A free form (501 mg) of (R)-3-[2-(2-hydroxymethylpyrrolidin-1-yl)ethyl]-5-methyl-2H-isoquinolin-1-one was measured in a reaction test tube, aqueous ethanol (4.3 mL, ethanol:water=8:1) was added and the mixture was completely dissolved by heating under reflux. Thereto was added aqueous phosphoric acid solution (2 mL, solution prepared by diluting commercially available 85% phosphoric acid (2.02 g) with the above-mentioned aqueous ethanol to scale up to 10 mL), and the mixture was stirred at room temperature for one day and left standing. The precipitate was collected by filtration. The obtained precipitate (302 mg) was measured in a reaction test tube, aqueous ethanol (2.4 mL, ethanol:water=6:1) was added, and the mixture was completely dissolved by heating under reflux. The mixture was stirred at room temperature for one day and left standing. The precipitate was collected by filtration and dried under reduced pressure at 50° C. for 5 hr to give the title compound (260 mg).

Workup

  1. dissolutionthe mixture was completely dissolved
  2. temperatureby heating
  3. temperatureunder reflux
  4. customprepared
  5. waitleft
  6. filtrationThe precipitate was collected by filtration
  7. customThe obtained precipitate (302 mg) was measured in a reaction test tube
  8. additionaqueous ethanol (2.4 mL, ethanol:water=6:1) was added
  9. dissolutionthe mixture was completely dissolved
  10. temperatureby heating
  11. temperatureunder reflux
  12. stirringThe mixture was stirred at room temperature for one day
  13. waitleft
  14. filtrationThe precipitate was collected by filtration
  15. customdried under reduced pressure at 50° C. for 5 hr

Sources & evidence

ORD record
ord-402944b832c94dee828bce60e1082000
Source dataset
uspto-grants-2012_11
Patent number
US08309573B2

Reaction notes

Loading…