Sulfuric acid magnesium salt (1:1) → HCID 68924573, compound

HRID 1788439Notes

Reaction equation

HRID 1788439 reaction equation
[O-]S([O-])(=O)=O.[Mg+2].[CH2:7]([O:9][C:10]([C:12]1[CH:40]=[CH:39][C:15]2[N:16]([CH:33]3[CH2:38][CH2:37][CH2:36][CH2:35][CH2:34]3)[C:17]([C:19]3[CH:24]=[CH:23][C:22]([N+:25]([O-])=O)=[C:21]([CH:28]([O:31][CH3:32])[O:29][CH3:30])[CH:20]=3)=[N:18][C:14]=2[CH:13]=1)=[O:11])[CH3:8]>CO.[Pd]>[CH2:7]([O:9][C:10]([C:12]1[CH:40]=[CH:39][C:15]2[N:16]([CH:33]3[CH2:34][CH2:35][CH2:36][CH2:37][CH2:38]3)[C:17]([C:19]3[CH:24]=[CH:23][C:22]([NH2:25])=[C:21]([CH:28]([O:29][CH3:30])[O:31][CH3:32])[CH:20]=3)=[N:18][C:14]=2[CH:13]=1)=[O:11])[CH3:8]

Participants

5

Reactant 2

HCID 24083Sulfuric acid magnesium salt (1:1)HCID 68921196HCID 68921196, compound

Product 1

HCID 68924573HCID 68924573, compound

Reagents, catalysts & solvents 2

HCID 23938PalladiumCatalystHCID 887MethanolSolvent2×

Procedure

In 20 mL methanol 100 mg of 10% Pd-C was pre-hydrogenated in the presence of 1 g MgSO4 at 30 psi for 15 minutes. Compound 354c (100 mg) dissolved in a solution of 20 mL of methanol containing 2 mL triethylamine, was added to the catalyst and the hydrogenation was continued for 30 minutes. The catalyst and the magnesium sulfate were filtered using Celite. The solution was evaporated to dryness and the oily residue was used immediately in the following step.

Workup

  1. additionwas added to the catalyst
  2. filtrationThe catalyst and the magnesium sulfate were filtered
  3. customThe solution was evaporated to dryness

Sources & evidence

ORD record
ord-99c1c52090f74667854cb9244b549d2b
Source dataset
uspto-grants-2009_03
Patent number
US07511145B2

Reaction notes

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