Sulfuric Acid → HCID 15078438, compound

HRID 345548Notes

Reaction equation

HRID 345548 reaction equation
[CH3:1][O:2][CH:3]1[C:8](OC)([O:9]C)[CH2:7][CH2:6][N:5]([CH2:13][C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)[CH2:4]1.S(=O)(=O)(O)O.C(=O)([O-])[O-].[Na+].[Na+]>>[CH3:1][O:2][CH:3]1[C:8](=[O:9])[CH2:7][CH2:6][N:5]([CH2:13][C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)[CH2:4]1

Participants

4

Reactant 3

HCID 1118Sulfuric AcidHCID 10340Sodium CarbonateHCID 15096756HCID 15096756, compound

Product 1

HCID 15078438HCID 15078438, compoundYield 98.6%

Procedure

A mixture of 38.1 parts of 3,4,4-trimethoxy-1-(phenylmethyl)piperidine and 1200 parts of sulfuric acid solution 1% was stirred and refluxed for 7 hours. The reaction mixture was allowed to cool overnight to room temperature and treated with sodium carbonate till a turbid solution was obtained. The product was extracted with 1,1'-oxybisethane. The extract was washed with water, dried, filtered and evaporated, yielding 28.8 parts (98.6%) of 3-methoxy-1-(phenylmethyl)-4-piperidinone as an oily residue (intermediate 60).

Workup

  1. temperaturerefluxed for 7 hours
  2. temperatureto cool overnight to room temperature
  3. customwas obtained
  4. extractionThe product was extracted with 1,1'-oxybisethane
  5. washThe extract was washed with water
  6. customdried
  7. filtrationfiltered
  8. customevaporated

Sources & evidence

ORD record
ord-cc93a6cf5c754dd98e0b1e6ce34d8e4e
Source dataset
uspto-grants-1991_10
Patent number
US05057525

Reaction notes

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