Methanol → HCID 178447306, compound

HRID 2060075Notes

Reaction equation

HRID 2060075 reaction equation
[C:1]([C@@H:4]([N:8]([C:27](=[O:32])[CH2:28][CH2:29][CH2:30][CH3:31])[CH2:9][C:10]1[CH:15]=[CH:14][C:13]([C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=2[C:22]2[NH:26][N:25]=[N:24][N:23]=2)=[CH:12][CH:11]=1)[CH:5]([CH3:7])[CH3:6])([OH:3])=[O:2].[OH-].[Mg+2:34].[OH-].CO>O>[Mg:34].[C:1]([C@@H:4]([N:8]([C:27](=[O:32])[CH2:28][CH2:29][CH2:30][CH3:31])[CH2:9][C:10]1[CH:11]=[CH:12][C:13]([C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=2[C:22]2[NH:23][N:24]=[N:25][N:26]=2)=[CH:14][CH:15]=1)[CH:5]([CH3:6])[CH3:7])([OH:3])=[O:2]

Participants

5

Reactant 3

HCID 887MethanolHCID 73981Magnesium HydroxideHCID 178447302HCID 178447302, compound

Product 1

HCID 178447306HCID 178447306, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

5 g of (S)-N-(1-carboxy-2-methyl-prop-1-yl)-N-pentanoyl-N-[2′-(1H-tetrazol-5-yl)-biphenyl-4-ylmethyl]-amine are added to a suspension of 0.666 g of magnesium hydroxide in 20 ml of water. 40 ml of methanol are added, then the mixture is stirred for 2 hours at room temperature and concentrated. The residue is dissolved in methanol, filtered through a hard filter, concentrated and evaporated with acetonitrile. The product is stirred with hot acetonitrile, filtered by suction at room temperature and dried in a high vacuum at 90° C. over night. (S)-N-(1-carboxy-2-methyl-prop-1-yl)-N-pentanoyl-N-[2′-(1H-tetrazol-5-yl)-biphenyl-4-ylmethyl]-amine magnesium salt is obtained as a white powder. Melting point: The sample becomes brownish upon heating and vitrifies towards 300° C.

Workup

  1. concentrationconcentrated
  2. dissolutionThe residue is dissolved in methanol
  3. filtrationfiltered through a hard filter
  4. concentrationconcentrated
  5. customevaporated with acetonitrile
  6. stirringThe product is stirred with hot acetonitrile
  7. filtrationfiltered by suction at room temperature
  8. customdried in a high vacuum at 90° C. over night

Sources & evidence

ORD record
ord-64092e60bfc44b17a2455cd0c2f27691
Source dataset
uspto-grants-2012_10
Patent number
US08278339B2

Reaction notes

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