HCID 131734559, compound → HCID 22872766, compound

HRID 593230Notes

Reaction equation

HRID 593230 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].[NH2:12][C@H:13]([C:19]([O-:21])=[O:20])[CH2:14][CH2:15][CH2:16][CH2:17][NH2:18].[Mg+2:22]

Participants

4

Reactant 1

HCID 131734559HCID 131734559, compound

Product 1

HCID 22872766HCID 22872766, compoundYield 196.5%

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 (1.00 g, 3.0 mmol) in methanol (5 mL) under nitrogen was treated with a solution of EPA (0.94 g, 3.1 mmol) in methanol (10 mL) containing alpha-D-tocopherol (100 mg) dissolved in ethyl acetate (0.5 mL), and stirred for 20 min, then most of the methanol was removed in vacuo and replaced with acetonitrile (20 mL). The mixture was stirred for 3 h, filtered, washed with acetonitrile, collected and dried in vacuo to afford 1.855 g (100%) of subject material as a pale beige solid.

Workup

  1. stirringstirred for 20 min
  2. custommost of the methanol was removed in vacuo
  3. stirringThe mixture was stirred for 3 h
  4. filtrationfiltered
  5. washwashed with acetonitrile
  6. customcollected
  7. customdried in vacuo

Sources & evidence

ORD record
ord-7ec175716ab64d77b2119f49ff85769d
Source dataset
uspto-grants-2016_01
Patent number
US09242008B2

Reaction notes

Loading…