Potassium Phosphate, Tribasic → HCID 69414650, compound

HRID 853050Notes

Reaction equation

HRID 853050 reaction equation
[Mg].[CH2:2]([C:4]1[C:12]2[N:11]3[C@H:13]([CH3:18])[CH2:14][NH:15][C:16](=[O:17])[C:10]3=[CH:9][C:8]=2[CH:7]=[CH:6][CH:5]=1)[CH3:3].[H][H].P([O-])([O-])([O-])=O.[K+].[K+].[K+]>CO>[CH2:2]([C:4]1[C:12]2[N:11]3[C@H:13]([CH3:18])[CH2:14][NH:15][C:16](=[O:17])[C@@H:10]3[CH2:9][C:8]=2[CH:7]=[CH:6][CH:5]=1)[CH3:3]

Participants

6

Reactant 4

HCID 62657Potassium Phosphate, TribasicHCID 5462224Magnesium2×HCID 11287627HCID 11287627, compoundHCID 178418361HCID 178418361, compound

Product 1

HCID 69414650HCID 69414650, compoundYield 97%

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

Magnesium turnings (87 mg, 3.6 mmol) were added to a solution of (R)-6-Ethyl-4-methyl-3,4-dihydro-2H-pyrazino[1,2-a]indol-1-one (82 mg, 0.36 mmol) in methanol (4 mL). After hydrogen gas started to evolve, the reaction mixture was kept at 10–20° C. and stirred for 2 h to dissolve the magnesium completely. Then the reaction mixture was poured onto 3 mL ice-cold 1 M aq. HCl, neutralized with 1 M aq. potassium phosphate solution (pH 6.85), and extracted with ethyl acetate. The organic layer was washed with brine, dried (MgSO4), and evaporated to yield the title compound (80 mg, 97%). White solid. ISP-MS: m/e=231.2 ([M+H]+).

Workup

  1. customwas kept at 10–20° C.
  2. extractionextracted with ethyl acetate
  3. washThe organic layer was washed with brine
  4. dry with materialdried (MgSO4)
  5. customevaporated

Sources & evidence

ORD record
ord-8709a1442f484665a4a21accd05f187e
Source dataset
uspto-grants-2007_08
Patent number
US07253281B2

Reaction notes

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