HCID 131734559, compound → HCID 22872766, compound

HRID 593229Notes

Reaction equation

HRID 593229 reaction equation
O.[NH2:2][C@H:3]([C:9]([O-:11])=[O:10])[CH2:4][CH2:5][CH2:6][CH2:7][NH2:8].[NH2:12][C@H:13]([C:19]([O-:21])=[O:20])[CH2:14][CH2:15][CH2:16][CH2:17][NH2:18].[Mg+2:22]>CO.C(OCC)(=O)C>[NH2:2][C@H:3]([C:9]([O-:11])=[O:10])[CH2:4][CH2:5][CH2:6][CH2:7][NH2:8].[Mg+2:22].[NH2:12][C@H:13]([C:19]([O-:21])=[O:20])[CH2:14][CH2:15][CH2:16][CH2:17][NH2:18]

Participants

4

Reactant 1

HCID 131734559HCID 131734559, compound

Product 1

HCID 22872766HCID 22872766, compoundYield 303.8%

Reagents, catalysts & solvents 2

HCID 887MethanolSolvent2×HCID 8857Ethyl AcetateSolvent

Conditions

Temperature
50 °C

Procedure

A warmed (50° C.) stirred suspension of magnesium bis-lysinate monohydrate (1.844 g, 5.0 mmol) in methanol (10 mL) under nitrogen was treated with a solution of EPA (3.63 g, 12 mmol) in methanol (10 mL) containing alpha-D-tocopherol (100 mg) dissolved in ethyl acetate (0.5 mL), stirred for 20 min, then the mixture was concentrated in vacuo and suspended in acetonitrile (50 mL). The suspension was stirred for 3 h, filtered, washed with acetonitrile, collected and dried in vacuo to afford 4.78 g (100%) of magnesium lysinate bis EPA as a white solid.

Workup

  1. stirringstirred for 20 min
  2. concentrationthe mixture was concentrated in vacuo
  3. stirringThe suspension was stirred for 3 h
  4. filtrationfiltered
  5. washwashed with acetonitrile
  6. customcollected
  7. customdried in vacuo

Sources & evidence

ORD record
ord-24ba460b4d2647bdbdfb5dd8a7651c8e
Source dataset
uspto-grants-2016_01
Patent number
US09242008B2

Reaction notes

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