MAGNESIUM SILICATE (synthetic) → HCID 19976958, compound

HRID 1742525Notes

Reaction equation

HRID 1742525 reaction equation
[OH:1][CH:2]([C:5]1[O:9][N:8]=[C:7]([C:10]2[CH:15]=[CH:14][C:13]([O:16][CH3:17])=[CH:12][CH:11]=2)[CH:6]=1)[CH2:3][CH3:4].C([O-])(=O)C.[Na+].[O-][Si]([O-])=O.[Mg+2].[Cr](Cl)([O-])(=O)=O.[NH+]1C=CC=CC=1>ClCCl>[CH3:17][O:16][C:13]1[CH:12]=[CH:11][C:10]([C:7]2[CH:6]=[C:5]([C:2](=[O:1])[CH2:3][CH3:4])[O:9][N:8]=2)=[CH:15][CH:14]=1

Participants

6

Reactant 4

HCID 61680MAGNESIUM SILICATE (synthetic)HCID 517045Sodium AcetateHCID 19976898HCID 19976898, compoundHCID 178418287HCID 178418287, compound

Product 1

HCID 19976958HCID 19976958, compound

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Procedure

Added to 160 ml of dichloromethane were 8.07 g (34.6 mmol) of 5-(1-hydroxypropyl)-3-(4-methoxyphenyl)isoxazole prepared in the above procedure (2), 4.83 g (58.9 mmol) of sodium acetate and 12.7 g of "Florisil" (trade mark, Wakojunyaku Inc.). While the resultant mixture was stirred vigorously, 12.7 g (58.9 mmol) pyridinium chlorochromate were added in small portions. After the mixture was stirred at room temperature for 4 hours, an insoluble material was filtered off and the solvent was distilled off. The residue was recrystallized from n-hexane, whereby 3-(4-methoxyphenyl)-5-propionylisoxazole was colorless crystals. Analytical results of the crystals obtained: Yield: 5.73 g (72%). Melting point: 135°-136° C.

Workup

  1. filtrationan insoluble material was filtered off
  2. distillationthe solvent was distilled off
  3. customThe residue was recrystallized from n-hexane, whereby 3-(4-methoxyphenyl)-5-propionylisoxazole
  4. customAnalytical results of the crystals
  5. customobtained

Sources & evidence

ORD record
ord-5206007324554f6bad71d50ac826e548
Source dataset
uspto-grants-1994_08
Patent number
US05338857

Reaction notes

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