Magnesium → HCID 117831023, compound

HRID 515893Notes

Reaction equation

HRID 515893 reaction equation
CC1C=CC(S([N:11]2[C@H:20]([CH2:21][CH2:22][CH2:23][N:24]3[CH2:29][CH2:28][O:27][CH2:26][CH2:25]3)[CH2:19][C:18]3[C:13](=[CH:14][CH:15]=[CH:16][CH:17]=3)[CH2:12]2)(=O)=O)=CC=1.[Mg]>CO>[N:24]1([CH2:23][CH2:22][CH2:21][C@@H:20]2[CH2:19][C:18]3[C:13](=[CH:14][CH:15]=[CH:16][CH:17]=3)[CH2:12][NH:11]2)[CH2:29][CH2:28][O:27][CH2:26][CH2:25]1

Participants

4

Reactant 2

HCID 5462224MagnesiumHCID 117830903HCID 117830903, compound

Product 1

HCID 117831023HCID 117831023, compound

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

To a solution of 1.50 g (3.62 mmol) of the compound obtained in Step E in 20 mL of anhydrous methanol there are added 2.0 g (82.3 mmol), in portions, of magnesium turnings. The batch is stirred in the presence of ultrasound for 96 hours. The reaction mixture is then filtered, the solid is washed several times with methanol, and the filtrate is concentrated to dryness. After purification by chromatography over silica gel using dichloromethane and ammonia-in-ethanol as eluants, the expected product is obtained in the form of an oil.

Workup

  1. filtrationThe reaction mixture is then filtered
  2. washthe solid is washed several times with methanol
  3. concentrationthe filtrate is concentrated to dryness
  4. customAfter purification by chromatography over silica gel

Sources & evidence

ORD record
ord-cad3ff23c8cb4962818fdc7e5d2fce23
Source dataset
uspto-grants-2015_08
Patent number
US09108983B2

Reaction notes

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